CN109020806A - A kind of recycling purification acetic acid extraction-entrainer - Google Patents
A kind of recycling purification acetic acid extraction-entrainer Download PDFInfo
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- CN109020806A CN109020806A CN201811282613.3A CN201811282613A CN109020806A CN 109020806 A CN109020806 A CN 109020806A CN 201811282613 A CN201811282613 A CN 201811282613A CN 109020806 A CN109020806 A CN 109020806A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
- C07C51/46—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation by azeotropic distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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Abstract
The present invention provides a kind of recycling purification acetic acid extraction-entrainer, including the following component of mass percent: acetates solvent, the hexamethylene of 15%-35% and the toluene of 10%-30% of 45%-65%.Preferably, extraction-entrainer is grouped as by the following group of mass percent: acetates solvent, the hexamethylene of 15%-35% and the toluene of 10%-30% of 45%-65%.It can not only be used for extractant but also as entrainer in the technical process of the extraction-entrainer extraction plus azeotropic distillation recycling purification acetic acid, after distillation operation separation will be not necessarily to after extraction-entrainer recycling, extraction process can be sent directly into and azeotropic distillation operates with, and separative efficiency is high.
Description
Technical field
The invention belongs to acetic acid recovery technical field of refinement, refine acetic acid extraction-azeotropic more particularly, to a kind of recycling
Agent.
Background technique
Acetic acid, that is, acetic acid is that a kind of structure is simple and very important organic mono carboxylic acid, is also important industrial chemicals,
It can be used for the chemicals such as synthesis for ethyl acetate, vinyl acetate, acetic anhydride, led in basic organic synthesis, chemical industry, medicine, fuel etc.
Domain is all widely used.The boiling point of acetic acid is higher than water, but close with water, and relative volatility is little, generally requires through rectifying
Method removes water, and acetic acid dehydration is frequently with conventional distillation or azeotropic distillation, and using conventional distillation equipment investment height, and energy consumption is high；
Azeotropic distillation changes the relative volatility of water and acetic acid, makes the number of plates needed for rectifying by making entrainer and water form azeotropic mixture
Reduce, reflux ratio reduces, save part energy consumption, but it is lower for acetate concentration in raw material when, the dosage of required entrainer increases
Add, rectifying column load increases, and system energy consumption is still very big.
It will extract in conjunction with azeotropic distillation, and extraction removing partial moisture first be carried out to a part of raw material, then carry out azeotropic essence
Entrainer dosage in azeotropic distillation can be substantially reduced by evaporating, and reduce azeotropic distillation rectifying column load and energy consumption, and can be by be processed
The ratio of the different adjustment extraction part materials of acetate concentration in raw material, so that whole equipment energy consumption substantially reduces.Extraction is together
It is respectively necessary for using extractant and entrainer in boiling rectifying, and since extraction phase finally will continue to enter in azeotropic distillation operation,
It just needs to separate extractant and entrainer when subsequent recovery recycles extractant and entrainer and utilization is separately recovered, make work
Skill process is more complicated, and system energy consumption increases, it is therefore desirable to a kind of acetic acid recovery purification extraction-entrainer, it can be simultaneously as extraction
It takes agent and entrainer to use, does not need to separate extractant and entrainer after recycling extraction-entrainer.
Summary of the invention
The problem to be solved in the present invention is to provide a kind of recycling to refine acetic acid extraction-entrainer, in extraction plus azeotropic essence
It evaporates and can not only be used for extractant in the technical process of recycling purification acetic acid but also as entrainer, by extraction-azeotropic after distillation operation
Without separation after agent recycling, extraction process can be sent directly into and azeotropic distillation operates with, and separative efficiency is high.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of recycling purification acetic acid extraction-azeotropic
Agent, including the following component of mass percent: the hexamethylene and 10%- of the acetates solvent of 45%-65%, 15%-35%
30% toluene.Wherein acetates solvent, which refers to be in a liquid state at normal temperatures and pressures in acetic ester compounds, can do the chemical combination of solvent
Object.Entrainer needs to be formed azeotropic mixture with water in distillation process in azeotropic distillation, and its boiling point need to have with the boiling point of water compared with
Big difference is in order to subsequent recovery entrainer, acetates solvent good entrainer when being rectifying spirit of vinegar.Extract foundation
Principle is the similar principle that mixes, and solubility is bigger between solvent similar in polarity, as the extractant of acetic acid, extraction-entrainer
Dichlorodiphenyl Acetate selectivity with higher is needed, hexamethylene is added and toluene adjusts extraction-entrainer polarity, makes extraction-azeotropic
Agent is bigger to the selectivity of acetic acid in dilute acetic acid, makes the extraction-entrainer that can form azeotropic mixture with water as azeotropic distillation effect
While rate high entrainer, and the extractant selectively high to acetic acid in dilute acetic acid.Using the extraction-entrainer simultaneously as
Extractant and entrainer in extraction plus azeotropic distillation recycling purification acetic acid technique, may be recovered after separating and recovering acetic acid,
It is directly used as extractant and entrainer after recycling, no longer needs to further separate it, simple process, low energy consumption.
In technical solution, it is preferred that extraction-entrainer is grouped as by the following group of mass percent: the vinegar of 45%-65%
The toluene of esters of gallic acid solvent, the hexamethylene of 15%-35% and 10%-30%.
In technical solution, it is preferred that acetates solvent is n-butyl acetate, isobutyl acetate, methyl acetate, acetic acid second
One of ester and isopropyl acetate or a variety of mixing.
In technical solution, it is preferred that acetates solvent includes n-butyl acetate, isobutyl acetate and methyl acetate.
In technical solution, it is preferred that the mass percent of acetates solvent is respectively as follows: the positive fourth of acetic acid of 17%-23%
The methyl acetate of ester, the isobutyl acetate of 22%-28% and 6%-14%.Present inventor through Thermodynamic Calculation,
Analysis, which is calculated, in conjunction with flowsheeting show that extraction-entrainer of said combination has optimal separative efficiency, acetic acid separated purification
Energy consumption is minimum, and the extraction after lot of experiments obtains each group subassembly of aforementioned proportion-entrainer actual separation effect
Fruit is best, and low energy consumption in entire acetic acid separated recovery process, and low energy consumption for entrainer recycling for extraction-.
The advantages and positive effects of the present invention are: the recycling refines acetic acid with extraction-entrainer in extraction plus azeotropic
It can be used as extractant and entrainer simultaneously in the technique of rectifying recycling purification acetic acid, it can step progress after the purification for completing acetic acid
The recycling and reusing of extraction-entrainer, no longer needs to be separated, simple process, energy saving, and the extraction-entrainer separation
It is high-efficient, reduce the energy consumption of entire acetic acid recovery process for refining.
Specific embodiment
Embodiments of the present invention are described further combined with specific embodiments below:
Embodiment one
Recycling purification acetic acid in the present embodiment is made of with extraction-entrainer the component of following mass fraction: 17%
N-butyl acetate, 22% isobutyl acetate and 14% methyl acetate, 20% hexamethylene and 27% toluene.
Treating material contains acetic acid 65%, water 35%.
Acetic acid recovery purification step is as follows:
1. the 30% of spirit of vinegar material is delivered at the top of extraction tower by feed pump, above-mentioned extraction-entrainer is from extraction
It takes tower bottom to enter and carries out normal pressure and temperature counter current contacting extracting operation, the mass ratio of extraction-entrainer and raw material is 2:1, extraction
Tower tower diameter is 300mm, theoretical cam curve 50；
2. the overhead extraction of extraction tower is acetic acid and extraction-entrainer, it is delivered in rectifying column through feed pump as charging,
Azeotropic distillation operation is carried out together with remaining 70% spirit of vinegar material, above-mentioned extraction-entrainer is added in the middle part of rectifying column,
Additional amount is 700kg/h, the top of the distillation column 800mm, and theoretical pedal number is 30-40, minimum reflux ratio 0.5-0.8, steam
Consumption is 1.0t/h, after azeotropic distillation operates, rectifying side take-off acetic acid, and concentration 99.6%；
3. the top of the distillation column extraction gas phase is mainly water, extraction-entrainer and a small amount of acetic acid, by it after condenser is cooling
It is sent into split-phase in phase-splitter, gained oil is mutually mainly extraction-entrainer and acetic acid, and oil is mutually sent into return tank, and a part passes through back
Stream blowback is flow in rectifying column, and another part is reused by pumping to be sent respectively to extraction tower, and water phase is mainly water, also contains part
Extraction-entrainer；
4. sending water phase obtained by split-phase into recovery tower, distillation operation is carried out, obtains extraction-entrainer in tower top, respectively
It send into rectifying column and extraction tower as extraction-entrainer recycling, the storage of tower reactor extracted waste water or discharge of recovery tower.
Embodiment two
Recycling purification acetic acid in the present embodiment is made of with extraction-entrainer the component of following mass fraction: 23%
N-butyl acetate, 28% isobutyl acetate and 10% methyl acetate, 15% hexamethylene and 24% toluene.
Treating material contains acetic acid 60%, water 40%.
Acetic acid recovery purification step is as follows:
1. the 25% of spirit of vinegar material is delivered at the top of extraction tower by feed pump, above-mentioned extraction-entrainer is from extraction
It takes tower bottom to enter and carries out normal pressure and temperature counter current contacting extracting operation, the mass ratio of extraction-entrainer and raw material is 2:1, extraction
Tower tower diameter is 300mm, theoretical cam curve 47；
2. the overhead extraction of extraction tower is acetic acid and extraction-entrainer, it is delivered in rectifying column through feed pump as charging,
Azeotropic distillation operation is carried out together with remaining 75% spirit of vinegar material, above-mentioned extraction-entrainer is added in the middle part of rectifying column,
Additional amount is 800kg/h, the top of the distillation column 800mm, and theoretical pedal number is 30-40, minimum reflux ratio 0.5-0.8, steam
Consumption is 1.3t/h, after azeotropic distillation operates, rectifying side take-off acetic acid, and concentration 99.6%；
3. the top of the distillation column extraction gas phase is mainly water, extraction-entrainer and a small amount of acetic acid, by it after condenser is cooling
It is sent into split-phase in phase-splitter, gained oil is mutually mainly extraction-entrainer and acetic acid, and oil is mutually sent into return tank, and a part passes through back
Stream blowback is flow in rectifying column, and another part is reused by pumping to be sent respectively to extraction tower, and water phase is mainly water, also contains part
Extraction-entrainer；
4. sending water phase obtained by split-phase into recovery tower, distillation operation is carried out, obtains extraction-entrainer in tower top, respectively
It send into rectifying column and extraction tower as extraction-entrainer recycling, the storage of tower reactor extracted waste water or discharge of recovery tower.
Embodiment three
Recycling purification acetic acid in the present embodiment is made of with extraction-entrainer the component of following mass fraction: 20%
N-butyl acetate, 25% isobutyl acetate and 10% methyl acetate, 20% hexamethylene and 25% toluene.
Treating material contains acetic acid 65%, water 35%.
Acetic acid recovery purification step is as follows:
1. the 40% of spirit of vinegar material is delivered at the top of extraction tower by feed pump, above-mentioned extraction-entrainer is from extraction
It takes tower bottom to enter and carries out normal pressure and temperature counter current contacting extracting operation, the mass ratio of extraction-entrainer and raw material is 2:1, extraction
Tower tower diameter is 300mm, theoretical cam curve 53；
2. the overhead extraction of extraction tower is acetic acid and extraction-entrainer, it is delivered in rectifying column through feed pump as charging,
Azeotropic distillation operation is carried out together with remaining 60% spirit of vinegar material, above-mentioned extraction-entrainer is added in the middle part of rectifying column,
Additional amount is 700kg/h, the top of the distillation column 800mm, and theoretical pedal number is 30-40, minimum reflux ratio 0.5-0.8, steam
Consumption is 1.6t/h, after azeotropic distillation operates, rectifying side take-off acetic acid, and concentration 99.6%；
3. the top of the distillation column extraction gas phase is mainly water, extraction-entrainer and a small amount of acetic acid, by it after condenser is cooling
It is sent into split-phase in phase-splitter, gained oil is mutually mainly extraction-entrainer and acetic acid, and oil is mutually sent into return tank, and a part passes through back
Stream blowback is flow in rectifying column, and another part is reused by pumping to be sent respectively to extraction tower, and water phase is mainly water, also contains part
Extraction-entrainer；
4. sending water phase obtained by split-phase into recovery tower, distillation operation is carried out, obtains extraction-entrainer in tower top, respectively
It send into rectifying column and extraction tower as extraction-entrainer recycling, the storage of tower reactor extracted waste water or discharge of recovery tower.
Several embodiments of the present invention are described in detail above, but the content is only preferable implementation of the invention
Example, should not be considered as limiting the scope of the invention.It is all according to all the changes and improvements made by the present patent application range
Deng should still be within the scope of the patent of the present invention.
Claims (5)
1. a kind of recycling refines acetic acid extraction-entrainer, it is characterised in that: including the following component of mass percent: 45%-
65% acetates solvent, the hexamethylene of 15%-35% and the toluene of 10%-30%.
2. recycling according to claim 1 refines acetic acid extraction-entrainer, it is characterised in that: such as by mass percent
Under group be grouped as: acetates solvent, the hexamethylene of 15%-35% and the toluene of 10%-30% of 45%-65%.
3. recycling according to claim 1 or 2 refines acetic acid extraction-entrainer, it is characterised in that: the acetates
Solvent is one of n-butyl acetate, isobutyl acetate, methyl acetate, ethyl acetate and isopropyl acetate or a variety of mixed
It closes.
4. recycling according to claim 3 refines acetic acid extraction-entrainer, it is characterised in that: the acetates are molten
Agent includes n-butyl acetate, isobutyl acetate and methyl acetate.
5. recycling according to claim 4 refines acetic acid extraction-entrainer, it is characterised in that: the acetates are molten
The mass percent of agent is respectively as follows: the n-butyl acetate of 17%-23%, the isobutyl acetate of 22%-28% and 6%-14%'s
Methyl acetate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811282613.3A CN109020806A (en) | 2018-10-31 | 2018-10-31 | A kind of recycling purification acetic acid extraction-entrainer |
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| CN201811282613.3A CN109020806A (en) | 2018-10-31 | 2018-10-31 | A kind of recycling purification acetic acid extraction-entrainer |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101312936A (en) * | 2005-09-23 | 2008-11-26 | Amt国际股份有限公司 | System and method for acetic acid dehydration |
| CN102153458A (en) * | 2011-02-28 | 2011-08-17 | 福州大学 | Method for recovering dilute acetic acid by virtue of extraction-azeotropic distillation of sec-butyl acetate |
| CN102267889A (en) * | 2011-06-03 | 2011-12-07 | 华东理工大学 | Method for recovering spirit of vinegar by combining extraction with azeotropic distillation |
| CN102344353A (en) * | 2010-08-04 | 2012-02-08 | 中国石油化工股份有限公司 | Method for dehydrating acetic acid |
| CN102432453A (en) * | 2011-10-31 | 2012-05-02 | 安丘市鲁安药业有限责任公司 | Process and equipment for purifying dilute acetic acid solution |
| CN102503802A (en) * | 2011-11-04 | 2012-06-20 | 南通醋酸纤维有限公司 | Acetic acid extracting agent |
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2018
- 2018-10-31 CN CN201811282613.3A patent/CN109020806A/en active Pending
Patent Citations (8)
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|---|---|---|---|---|
| CN101312936A (en) * | 2005-09-23 | 2008-11-26 | Amt国际股份有限公司 | System and method for acetic acid dehydration |
| CN102344353A (en) * | 2010-08-04 | 2012-02-08 | 中国石油化工股份有限公司 | Method for dehydrating acetic acid |
| CN102153458A (en) * | 2011-02-28 | 2011-08-17 | 福州大学 | Method for recovering dilute acetic acid by virtue of extraction-azeotropic distillation of sec-butyl acetate |
| CN102267889A (en) * | 2011-06-03 | 2011-12-07 | 华东理工大学 | Method for recovering spirit of vinegar by combining extraction with azeotropic distillation |
| CN102838470A (en) * | 2011-06-20 | 2012-12-26 | 逸盛大化石化有限公司 | Energy saving method for acetic acid dehydration column |
| CN102432453A (en) * | 2011-10-31 | 2012-05-02 | 安丘市鲁安药业有限责任公司 | Process and equipment for purifying dilute acetic acid solution |
| CN102503802A (en) * | 2011-11-04 | 2012-06-20 | 南通醋酸纤维有限公司 | Acetic acid extracting agent |
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