CN104447200B - For separating ethylene glycol and the rectificating method of 1,2-butanediol - Google Patents
For separating ethylene glycol and the rectificating method of 1,2-butanediol Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- 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
- C07C29/82—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by azeotropic distillation
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Abstract
The present invention relates to a kind of for separating ethylene glycol and 1, the rectificating method of 2 butanediols, mainly solve prior art separation ethylene glycol and 1, during 2 butanediol, rectification separation process long flow path, the technical problem that investment is big, energy consumption is high.The present invention is by using following steps: containing ethylene glycol and 1, the raw material of 2 butanediols enters rectifying tower with bulkhead bulkhead section feeding side (I), ethylene glycol therein forms azeotropic mixture with the fresh entrainer added from phase separator, steam from tower top, upper strata richness entrainer after condensed split-phase returns the public rectifying section of rectifying tower with bulkhead (III) mutually and continues to participate in azeotropic, lower floor's richness ethylene glycol phase returns to bulkhead section feeding side (I) and continues refined after mixing with raw material, separated, ethylene glycol is obtained at bulkhead section feeding side bottom, 1 is obtained in bulkhead section opposite side (II) bottom, the technical scheme of 2 butanediols preferably solves above-mentioned technical problem, can be used for separating ethylene glycol and 1, in the commercial production of 2 butanediols.
Description
Technical field
The present invention relates to a kind of for separating ethylene glycol and the rectificating method of 1,2-butanediol.
Background technology
Ethylene glycol is a kind of important basic organic chemical industry raw material, is mainly used in producing poly-to benzene with p-phthalic acid copolymerization
Naphthalate (PET).Additionally, ethylene glycol can also be used for producing antifreezing agent, lubricant, plasticizer, non-ionic surface work
Property agent and explosive etc., purposes is widely.China is the consumption big country of ethylene glycol, and the yield of current domestic ethylene glycol is far from full
Foot demand, has good development prospect.
1,2-butanediol is also a kind of Organic Chemicals, owing to its viscosity and freezing point are the lowest, is mainly used as polyester
The diol monomer modified with polyurethane resin, and it is used as the plasticizer production raw material of polyvinyl chloride resin.Additionally, 1,2-butanediol is also
Can be used for producing other fine chemicals such as the wetting agent of cosmetics, pesticide stabilizer, medicine, purposes is the most quite varied.
With Semen Maydis as raw material, through bioconversion can produce ethylene glycol, 1,2-PD, 1, the polyhydric alcohol such as 2-butanediol,
Wanting to obtain various high-purity chemical industry alcohol product, need to solve because of ethylene glycol and 1,2-butanediol boiling point difference is the least, uses common
Rectification Need Hierarchy Theory plate number is many, invest big technical problem.
In the last few years, rely on the coal resources of China's abundant, with coal as primary raw materials, couple producing oxalic ester through synthesis gas,
A very wide range of concern is received again by the process route of producing ethylene glycol from hydrogenation of oxalic ester.At hydrogenation of oxalate for preparing ethylene glycol
Containing the 1,2-PD and 1 the most close with ethylene glycol boiling point in product, 2-butanediol, especially 1,2-butanediol,
Closest with ethylene glycol boiling point, it is most difficult to separate.Therefore, wanting to obtain high-purity ethylene glycol product, how separation removal is therein
1,2-butanediol is the key of problem.
CN 101928201 proposes by saponification, go methanol, hydrogenation reaction, three-tower rectification and adsorption treatment
Technical scheme purify synthesis gas glycol rude products.But, in three-tower rectification purification process, 1,2-butanediol and second two
Alcohol generation azeotropic, the two be kept completely separate the most unrealized, also bring the product of ethylene glycol to lose, reduce product yield, with
Time also cause the technical disadvantages such as long flow path, investment are big.
Azeotropic distillation is a kind of special extract rectification process, is mainly used in azeotropic mixture and the separation of the nearly thing that boils.It is by quilt
Separation mixture adds score from low the 3rd component (also referred to as entrainer) of component volatilization degree, make this component with in separated object system
One or more components form new azeotropic mixture, thus change the relative volatility between separation component, and then by common essence
The method evaporated is separated, and is a kind of important industrial process.
US 4,966,658 proposition ethylbenzene, 3-heptanone, diisobutyl ketone etc. are as entrainer, the method using azeotropic distillation
Separating ethylene glycol and 1,2-butanediol, 1,3 butylene glycol, the number of theoretical plate of rectifying column is 30.Azeotropic essence involved in this patent
The process that evaporates needs harsher operating condition just can obtain the ethylene glycol of higher degree, such as, need the highest vacuum
(8KPa), or under relatively rough vacuum, need the time of staying (5～12hr) grown very much, and the ethylene glycol obtained still contains
A small amount of 1,2-butanediol or entrainer etc., to obtain the ethylene glycol of top grade product, still need to remove above-mentioned impurity further.
Due to during azeotropic distillation, the tower top azeotropic mixture rich product after split-phase mutually in existence more or less a small amount of
Entrainer or other raw material components, therefore, in traditional azeotropic distillation technique, in addition to azeotropy rectification column, generally also need to one
Seat product purification tower, just can obtain high-purity product, the most also bring long flow path, investment after being separated further by above-mentioned impurity
Greatly, the shortcoming that energy consumption is high.
The concept source of rectifying tower with bulkhead is in the complete thermal coupled rectifying tower of Petlyuk, and it is by a rectifying column
Vertical partition plate or the dividing plate at band angle of inclination of one or more certain length are installed, use a set of vaporization and condensation system, simultaneously
The product of isolated three kinds or more.Due to the most a set of vaporization and condensation system, and avoid employing multitower rectification
Time the remixing of intermediate component, therefore rectifying tower with bulkhead is than traditional distillation technology investment reduction 20～30%, energy consumption reduce by 10～
40%。
Rectifying tower with bulkhead is mainly used in multi-component conventional rectification separation process, in the last few years, by rectifying tower with bulkhead and its
During the application that its separation process combines also is evolving.EP 0126288 and US 8,178,060 all proposes bulkhead rectification
Tower is applied to reactive distillation processes；US 7,556,717 proposes rectifying tower with bulkhead is applied to extracting rectifying process, such as, be used for
The extracting of butadiene, energy consumption reduction by 16%, equipment cost reduction by 20%, on-the-spot cost reduce by 10%；CN 101028987 proposes to divide
Wall rectifying column is applied to the process of separation of extractive distillation propylene and propane, and energy consumption reduces by 30%, and running cost and equipment cost also have
Substantially reduce；CN 102040542 proposes that rectifying tower with bulkhead is applied to azeotropic distillation and reclaims the acetonitrile in waste water, and energy consumption reduces
35%, wherein the structure of divided wall column belongs to traditional form, i.e. vertical partition plate is positioned at the middle part of rectifying tower with bulkhead.Therefore, by bulkhead essence
Evaporate tower and be applied to azeotropic distillation separation ethylene glycol and 1, during 2-butanediol, traditional azeotropy rectification column and product can be replaced
Treating column, it is achieved the effect of two tower unifications, has 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 separation ethylene glycol and 1, during 2-butanediol, and rectification separation process flow process
Technical problem long, that investment is big, energy consumption is high, it is provided that one is used for separating ethylene glycol and 1, the rectificating method of 2-butanediol, is somebody's turn to do
Method has the advantage that flow process is short, small investment, energy consumption are low.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is as follows: one is used for separating ethylene glycol and 1,
The rectificating method of 2-butanediol, comprises the following steps: containing ethylene glycol and 1, the raw material of 2-butanediol enters rectifying tower with bulkhead bulkhead
Section feeding side (I), ethylene glycol therein forms azeotropic mixture with the fresh entrainer added from phase separator, steams from tower top, through cold
Upper strata richness entrainer after solidifying split-phase returns the public rectifying section of rectifying tower with bulkhead (III) mutually and continues to participate in azeotropic, lower floor's richness second two
Alcohol phase returns to bulkhead section feeding side (I) and continues refined after mixing with raw material, separated, obtains in bottom, bulkhead section feeding side (I)
Ethylene glycol, obtains 1 in bulkhead section opposite side (II) bottom, 2-butanediol.
In technique scheme, rectifying tower with bulkhead includes bulkhead section feeding side (I), bulkhead section opposite side (II) and public essence
The section of evaporating (III), the dividing plate of bulkhead section is along the axially vertical installation of tower or not along the axially vertical installation of tower；Rectifying tower with bulkhead have 30～
60 pieces of theoretical plates, bulkhead section has 20～50 pieces of theoretical plates, and public rectifying section has 10～30 pieces of theoretical plates；Containing ethylene glycol and 1,2-fourth
The raw material of glycol enters from the top of bulkhead section feeding side (I), and charging aperture is positioned at the 1st ~ 15 piece from demarcation strip top down number
Theoretical plate；Fresh entrainer adds from phase separator, enters back into rectifying tower with bulkhead and participates in azeotropic, and charging aperture is positioned at public rectifying section
Top, from top to bottom the 1st ~ 10 piece of theoretical plate of number；After entrainer forms azeotropic mixture with ethylene glycol, from the tower top of rectifying tower with bulkhead
Steaming, enter phase separator after overhead condenser cools down, the upper strata richness entrainer after layering returns the public essence of rectifying tower with bulkhead mutually
The section of evaporating continues to participate in azeotropic, and lower floor's richness ethylene glycol phase returns to bulkhead section feeding side and continues refined after mixing with raw material；Bulkhead rectification
The operation pressure of tower is calculated as 50～101.3KPa with absolute pressure；Tower top reflux ratio by weight is 10～40；Public rectifying section
It is 0.33～3 that liquid phase enters the liquid phase weight ratio of bulkhead section feeding side (I) and bulkhead section opposite side (II)；Resolution element in tower
It it is the combination of column plate, filler or column plate and filler；Entrainer and the mol ratio 0.1 ~ 10:1 of ethylene glycol, the knot of entrainer in raw material
Structure formula is:
In formula: R1For H atom or the alkyl containing 1～2 carbon atom, R2For H atom or containing the alkyl of 1～2 carbon atom,
R3For H atom or the alkyl containing 1～5 carbon atom, R4For H atom or the alkyl containing 1～5 carbon atom.Separated, at bulkhead
Bottom, section feeding side (I) obtains ethylene glycol, obtains 1 in bulkhead section opposite side (II) bottom, 2-butanediol.
Due to the method that have employed azeotropic distillation, it is to avoid employing conventional distillation method separation ethylene glycol and 1,2-butanediol
Time need the highest reflux ratio and number of theoretical plate, reduce equipment investment and energy consumption, improve product yield.Simultaneously as adopt
With rectifying tower with bulkhead for the two azeotropic separation, it is to avoid use the tradition azeotropic distillation to need to first pass through azeotropic distillation when separating
Tower removing 1,2-butanediol, again by product purification tower removing trace entrainer two tower process flow processs, namely by use one
Seat rectifying tower with bulkhead realizes the effect of two tower unifications, simplifies technological process.The present invention passes through Optimizing Technical, and it is suitable to use
Rectifying tower with bulkhead structure, by reducing a rectifying column and a set of vaporization and condensation system, serve reduction equipment cost, operation
Cost and the effect of reduction energy consumption, achieve unforeseeable technique effect compared to existing technology.Although CN 102040542
Proposing that rectifying tower with bulkhead is applied to azeotropic distillation and reclaim the acetonitrile in waste water, wherein the structure of divided wall column belongs to traditional form,
I.e. vertical partition plate is positioned at the technical scheme at middle part of rectifying tower with bulkhead, but separate due to it is acetonitrile and water, both physics
Character difference is relatively big, and material to be separated in the present invention is ethylene glycol and 1,2-butanediol, and both physical propertys connect very much
Closely, those skilled in the art can not expect being used for rectifying tower with bulkhead ethylene glycol and 1, the separation of 2-butanediol, can also take simultaneously
Obtaining separating effect well, the present invention, under identical raw material condition and ethylene glycol product require, uses the present invention to carry out second two
Alcohol and 1, the separating experiment of 2-butanediol, achieve unforeseeable technique effect, the more traditional two tower azeotropic distillation techniques of energy consumption
More than 13% can be reduced.
Accompanying drawing explanation
Fig. 1 is the rectificating method process chart for separating ethylene glycol and 1,2-butanediol involved in the present invention
Fig. 2 is the traditional azeotropic distillation process chart separated with 1,2-butanediol for ethylene glycol
Fig. 3 is the conventional distillation process chart separated with 1,2-butanediol for ethylene glycol
Fig. 4 is the conventional rectifying tower with bulkhead process chart separated with 1,2-butanediol for ethylene glycol
Fig. 5 is the rectifying tower with bulkhead process chart containing public stripping section separated with 1,2-butanediol for ethylene glycol
In Fig. 1, C101 be rectifying tower with bulkhead, C102 be phase separator, E101 be that rectifying tower with bulkhead overhead condenser, E102 are
The tower reactor reboiler of rectifying tower with bulkhead bulkhead section feeding side, E103 are the tower reactor reboiler of rectifying tower with bulkhead bulkhead section opposite side；I
For bulkhead section feeding side, II be bulkhead section opposite side, III be public rectifying section；Wherein material inlet is positioned at the top of I, richness altogether
Boiling agent phase import is positioned at the top of III.Logistics 101 is to be fresh azeotropic containing ethylene glycol and the raw material of 1,2-butanediol, logistics 102
Agent, logistics 103 be the ethylene glycol after separating, logistics 104 be entrainer and the azeotropic mixture of ethylene glycol formation, without 1,2-fourth two
Alcohol, logistics 105 are the upper strata richness entrainer phase after azeotropic mixture layering, logistics 106 is the lower floor's richness ethylene glycol after azeotropic mixture is layered
Phase, logistics 107 are the 1,2-butanediol after separating.
In Fig. 2, C201 be azeotropy rectification column, C202 be product purification tower, C203 be phase separator, E201 be azeotropy rectification column
Overhead condenser, E202 be azeotropy rectification column tower reactor reboiler, E203 be product purification column overhead condenser, E204 be product essence
Tower tower reactor reboiler processed；Logistics 201 is to be fresh entrainer, logistics containing ethylene glycol and the raw material of 1,2-butanediol, logistics 202
203 for having neither part nor lot in the 1,2-butanediol of azeotropic, logistics 204 be the azeotropic mixture that formed with ethylene glycol of entrainer, logistics 205 be azeotropic
Upper strata richness entrainer phase, logistics 206 after thing layering are the lower floor's richness ethylene glycol phase after azeotropic mixture layering, logistics 207 is rich second
A small amount of entrainer, logistics 208 in two alcohol phase are ethylene glycol.
In Fig. 3, C301 be common rectifying tower, E301 be common rectifying tower overhead condenser, E302 be common rectifying tower tower
Still reboiler；Logistics 301 be raw material, logistics 302 containing ethylene glycol with 1,2-butanediol be the overhead after separating, logistics
303 is the tower reactor distillation after separating
In Fig. 4, C401 is conventional rectifying tower with bulkhead, C402 is phase separator, E401 is rectifying tower with bulkhead overhead condenser,
E402 is rectifying tower with bulkhead tower reactor reboiler；V be bulkhead section feeding side, VI be bulkhead section opposite side, VII be public rectifying section,
VIII is public stripping section；Wherein material inlet is positioned at the middle and upper part of V, rich entrainer phase import is positioned at the top of VII, side line produces
Product outlet is positioned at the middle and lower part of VI.Logistics 401 be containing ethylene glycol and the raw material of 1,2-butanediol, logistics 402 be fresh entrainer,
The azeotropic mixture that logistics 403 is entrainer to be formed with ethylene glycol, without 1, upper for after azeotropic mixture layering of 2-butanediol, logistics 404
The rich entrainer phase of layer, logistics 405 are the lower floor's richness ethylene glycol phase after azeotropic mixture layering, logistics 406 is that the tower reactor after separating distillates
Thing, logistics 407 are the side stream after separating.
In Fig. 5, C501 be the rectifying tower with bulkhead with public stripping section, C502 be phase separator, E501 be that rectifying tower with bulkhead divides
The overhead condenser of wall section feeding side, E102 be the overhead condenser of rectifying tower with bulkhead bulkhead section opposite side, E103 be bulkhead essence
Evaporate tower tower reactor reboiler；X be bulkhead section feeding side, XI be bulkhead section opposite side, XII be public stripping section；Wherein material inlet
Be positioned at the middle and lower part of X, rich entrainer phase import is positioned at the top of XI.Logistics 501 be the raw material containing ethylene glycol and 1,2-butanediol,
Logistics 502 be fresh entrainer, logistics 503 be the overhead of bulkhead section feeding side, logistics 504 be entrainer and ethylene glycol
The azeotropic mixture formed, without 1,2-butanediol, logistics 505 are common for the upper strata richness entrainer phase after azeotropic mixture layering, logistics 506
Lower floor's richness ethylene glycol phase, logistics 507 after boiling thing layering are the tower reactor distillation after separating.
Below by embodiment, the invention will be further elaborated.
Detailed description of the invention
[embodiment 1]
Rectifying tower with bulkhead tower body as shown in Figure 1, total number of theoretical plate is 60, bulkhead section number of theoretical plate 40, bulkhead section every
Plate is positioned axially, and material inlet is positioned at the 10th piece of theoretical plate of bulkhead section side number from top to bottom, and entrainer import is positioned at
At 5th piece of theoretical plate of public rectifying section number from top to bottom.Percentage by weight consists of ethylene glycol 85%, 1,2-butanediol 15%
Raw material adds from material inlet, entrainer (substituent R1、R2、R3And R4It is respectively as follows :-H ,-H ,-CH3、-(CH2)4CH3) from azeotropic
Agent import adds, and entrainer is 1.5:1 with the mol ratio of ethylene glycol in raw material, and the operation pressure of rectifying tower with bulkhead is normal pressure, returns
Flow ratio is 15, and liquid phase distribution 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, from the ethylene glycol of bulkhead section feeding side tower reactor extraction purity by weight percentage after separation
Be 99.9%, from the 1 of bulkhead section opposite side tower reactor extraction, 2-butanediol purity by weight percentage is 99.9%, total energy consumption
It is 4.785 × 103Kilojoule/(kilogram × hour), relatively comparative example 1 reduce 13.8%.
[embodiment 2]
Rectifying tower with bulkhead tower body as shown in Figure 1, total number of theoretical plate is 45, bulkhead section number of theoretical plate 30, bulkhead section every
Plate is positioned axially, and material inlet is positioned at the 8th piece of theoretical plate of bulkhead section side number from top to bottom, and entrainer import is positioned at public affairs
Altogether at the 5th piece of theoretical plate of rectifying section number from top to bottom.Percentage by weight consist of ethylene glycol 60%, 1,2-butanediol 40% former
Expect to add from material inlet, entrainer (substituent R1、R2、R3And R4It is respectively as follows :-H ,-H ,-CH3、-(CH2)4CH3) from entrainer
Import adds, and entrainer is 1.5:1 with the mol ratio of ethylene glycol in raw material, and the operation pressure of rectifying tower with bulkhead is 50KPa, backflow
Ratio is 25, and liquid phase distribution 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, separately
The temperature of side is 183 DEG C, after separation from the ethylene glycol of bulkhead section feeding side tower reactor extraction purity is by weight percentage
99.8%, from the 1 of bulkhead section opposite side tower reactor extraction, 2-butanediol purity by weight percentage is 99.9%, and total energy consumption is
4.936×103Kilojoule/(kilogram × hour).
[comparative example 1]
To use logistics same as in Example 1 be raw material, uses entrainer same as in Example 1, stream as shown in Figure 2
Journey, azeotropy rectification column number of theoretical plate is 20, entrainer is 1.5:1 with the mol ratio of ethylene glycol in raw material, operation 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, behaviour
Being normal pressure as pressure, tower top temperature is 166 DEG C, bottom temperature is 198 DEG C.From the 1,2-of azeotropy rectification column tower reactor extraction after separation
Butanediol purity by weight percentage is 99.9%, from the ethylene glycol of product purification tower tower reactor extraction by weight percentage
Purity be 99.9%, total energy consumption is 5.551 × 103Kilojoule/(kilogram × hour), relatively embodiment 1 add 16.0%, and increase
Add 1 rectifying column and 1 overhead condenser, add equipment investment.
[comparative example 2]
Using logistics same as in Example 1 is raw material, flow process as shown in Figure 3, the tower number of theoretical plate of common rectifying tower
Be 120, reflux ratio be 130, operation pressure is normal pressure, and tower top temperature is 166 DEG C, bottom temperature is 196 DEG C.Tower top after separation
Distillation by weight percentage consist of 1,2-butanediol purity 83.6%, ethylene glycol 16.7%, second two in tower reactor distillation
Alcohol purity by weight percentage is 99.9%, although use conventional distillation method relatively embodiment 1, embodiment 2 to decrease 1
Tower reactor reboiler, but it is difficult to ethylene glycol and 1, being kept completely separate of 2-butanediol, and have lost a large amount of ethylene glycol, this contrast
Example total energy consumption is 6.129 × 103Kilojoule/(kilogram × hour), relatively embodiment 1 add 28.1%.
[comparative example 3]
Use raw material same as in Example 1 and entrainer, flow process as shown in Figure 4, total theoretical plate of rectifying tower with bulkhead
Number is 60, and bulkhead section number of theoretical plate 40, the number of theoretical plate of public rectifying section and public stripping section is 10, and side line discharge is positioned at
At 20th piece of theoretical plate of bulkhead section number from top to bottom, 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 distillation after separation: ethylene glycol 91.3%, 1,2-butanediol 8.7%；
Consisting of by weight percentage in side stream: ethylene glycol 34.6%, 1,2-butanediol 65.4%, unrealized divides completely
From.
[comparative example 4]
Use raw material same as in Example 1 and entrainer, flow process as shown in Figure 5, total theoretical plate of rectifying tower with bulkhead
Number is 60, bulkhead section number of theoretical plate 40, and material inlet is positioned at the 30th piece of theoretical plate of bulkhead section side number from top to bottom, azeotropic
Agent import is positioned at the 5th piece of theoretical plate of bulkhead section opposite side number from top to bottom, and other condition is with embodiment 1；Tower top bulkhead section
The temperature of charging side is 166 DEG C, the temperature of opposite side is 166 DEG C, and bottom temperature is 198 DEG C, the overhead after separation
In consisting of by weight percentage: ethylene glycol 89.3%, entrainer 10.7%；In tower reactor distillation by weight percentage
Consist of: ethylene glycol 87.2%, 1,2-butanediol 12.8%, separating effect is inconspicuous.
Claims (6)
1. one kind is used for separating ethylene glycol and 1, the rectificating method of 2-butanediol, comprises the following steps: containing ethylene glycol and 1,2-fourth
The raw material of glycol enters rectifying tower with bulkhead bulkhead section feeding side (I), ethylene glycol therein and the fresh azeotropic added from phase separator
Agent forms azeotropic mixture, steams from tower top, and the upper strata richness entrainer after condensed split-phase returns the public rectifying section of rectifying tower with bulkhead mutually
(III) continuing to participate in azeotropic, lower floor's richness ethylene glycol phase returns to bulkhead section feeding side (I) and continues refined, through dividing after mixing with raw material
From, obtain ethylene glycol in bottom, bulkhead section feeding side (I), obtain 1 in bulkhead section opposite side (II) bottom, 2-butanediol；Bulkhead
Rectifying column has 30～60 pieces of theoretical plates, and bulkhead section has 20～50 pieces of theoretical plates, and public rectifying section has 10～30 pieces of theoretical plates；Point
Wall rectifying column tower top reflux ratio by weight is 10～40；The liquid phase of the public rectifying section of rectifying tower with bulkhead (III) enters bulkhead
The liquid phase weight ratio of section feeding side (I) and bulkhead section opposite side (II) is 0.33～3.
The most according to claim 1 for separating ethylene glycol and 1, the rectificating method of 2-butanediol, it is characterised in that bulkhead
Rectifying column includes bulkhead section feeding side (I), bulkhead section opposite side (II) and public rectifying section (III), and the dividing plate of bulkhead section is along tower
Axially vertical installation or not along the axially vertical installation of tower.
The most according to claim 1 for separating ethylene glycol and 1, the rectificating method of 2-butanediol, it is characterised in that raw material
Entering from the top of bulkhead section feeding side (I), charging aperture is positioned at the 1st～15 piece of theoretical plate from demarcation strip top down number.
The most according to claim 1 for separating ethylene glycol and 1, the rectificating method of 2-butanediol, it is characterised in that azeotropic
Upper strata richness entrainer after thing layering enters from the top of public rectifying section (III), and charging aperture is positioned at public rectifying section (III)
1st～10 piece of theoretical plate of number from top to bottom.
The most according to claim 1 for separating ethylene glycol and 1, the rectificating method of 2-butanediol, it is characterised in that bulkhead
The operation pressure of rectifying column is calculated as 50～101.3KPa with absolute pressure.
The most according to claim 1 for separating ethylene glycol and 1, the rectificating method of 2-butanediol, it is characterised in that in tower
Resolution element be the combination of column plate, filler or column plate and filler.
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| CN107001206B (en) * | 2014-12-18 | 2021-04-23 | 国际壳牌研究有限公司 | Process for separating diols |
| BR112017021550B1 (en) * | 2015-04-07 | 2021-07-13 | Shell Internationale Research Maatschappij B.V. | PROCESS FOR THE SEPARATION OF MONOETHYLENEGLYCOL (MEG) AND 1,2-BUTANEDIOL (1,2-BDO) |
| 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 |
| CN109771980B (en) * | 2018-12-23 | 2021-04-13 | 中国科学院山西煤炭化学研究所 | Heterogeneous azeotropic rectification method for separating mixture of 2-pentanone, 4-heptanone, water and carbon dioxide |
| 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 |
| CN111518593B (en) * | 2020-04-23 | 2022-08-23 | 河北工业大学 | Method for primarily separating byproduct mixed alcohol in coal indirect liquefaction process |
| CN114712883B (en) * | 2022-04-21 | 2023-06-23 | 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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| CN103193594A (en) * | 2012-01-10 | 2013-07-10 | 中国石油化工股份有限公司 | Method for separating ethylene glycol and 1, 2-butanediol |
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| US4966658A (en) * | 1989-12-27 | 1990-10-30 | Lloyd Berg | Recovery of ethylene glycol from butanediol isomers by azeotropic distillation |
| CN103193594A (en) * | 2012-01-10 | 2013-07-10 | 中国石油化工股份有限公司 | Method for separating ethylene glycol and 1, 2-butanediol |
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