CN105381624A - Azeotropy rectification method-based acetic acid recovery device and method - Google Patents
Azeotropy rectification method-based acetic acid recovery device and method Download PDFInfo
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- CN105381624A CN105381624A CN201510820644.XA CN201510820644A CN105381624A CN 105381624 A CN105381624 A CN 105381624A CN 201510820644 A CN201510820644 A CN 201510820644A CN 105381624 A CN105381624 A CN 105381624A
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- acetic acid
- azeotropy rectification
- rectification column
- entrainer
- input port
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/36—Azeotropic distillation
-
- 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
Abstract
The invention relates to an azeotropy rectification method-based acetic acid recovery device and method. The device comprises an acetic acid recovery device body with an azeotropy rectification tower (1), wherein the middle part of the tower (1) is provided with a dilute acetic acid input end opening, the top of the azeotropy rectification tower (1) is provided with an entrainer input end opening, and the side face part of the bottom of the azeotropy rectification tower (1) is provided with an acetic acid output end opening. By inputting dilute acetic acid by the middle part of the azeotropy rectification tower (1) and inputting an entrainer by the top of the azeotropy rectification tower (1), water in the dilute acetic acid and the entrainer are mixed to form mixed liquor with a boiling point greatly different from that of acetic acid, and inputting the dilute acetic acid directly from the top of the azeotropy rectification tower (1) is not needed any more, so the tower diameter of the rectification tower, a number of needed tower plates and a reflux ratio parameter are optimized, and the amount of hot steam is saved.
Description
One, technical field
The present invention relates to a kind of acetic acid recovery device and method, especially a kind of acetic acid recovery device and method based on azeotropic distillation.
Two, background technology
Acetic acid is a kind of important Organic Chemicals, also be one of methyl alcohol major downstream derivative products, be widely used in basic organic synthesis, medicine, agricultural chemicals, printing and dyeing, light textile, food, make paint, in many technical fields such as adhesive, therefore acetic acid recovery device and method is a kind of important light industry process and device, method now for acetic acid recovery mainly contains rectification method, extraction, absorption method, membrane separation process and esterification process, main employing be rectification method, acetic acid is obtained at the bottom of tower, but because both acetic acid and water boiling point is close, relative volatility is little, belong to highly imperfect system, obtain high-purity acetic acid, conventional distillation is adopted to need very large tower diameter and a lot of column plates and very large reflux ratio to be generally reflux ratio up to 20-30, at substantial steam increases by this, waste the energy, as shown in Figure 1, 11-rectifying column, 12-primary cooler, 13-return tank, the elementary reboiler of 14-, 15-reflux pump.
Three, summary of the invention
In order to overcome above-mentioned technical disadvantages, the object of this invention is to provide a kind of acetic acid recovery device and method based on azeotropic distillation, therefore optimizing rectifying column tower diameter, the required number of plates and reflux ratio parameter, saved vapours amount.
For achieving the above object, the technical scheme that the present invention takes is: include the acetic acid recovery device body with azeotropy rectification column, the pars intermedia of azeotropy rectification column be provided with spirit of vinegar input port, be provided with at the top of azeotropy rectification column entrainer input port and the tower bottom side of azeotropy rectification column face is provided with the output port of acetic acid.
Owing to devising acetic acid recovery device body, by entering spirit of vinegar at azeotropy rectification column pars intermedia, entering entrainer at the top of azeotropy rectification column, the water in spirit of vinegar and entrainer can be made to be mixed to form the mixed liquor had a long way to go with acetic acid boiling point, no longer directly enter spirit of vinegar from azeotropic distillation top of tower, therefore optimize rectifying column tower diameter, the required number of plates and reflux ratio parameter, save vapours amount.
The present invention devises, and the mode being mixed to form the mixed liquor had a long way to go with acetic acid boiling point according to the water made in spirit of vinegar and entrainer is carried out the material input mouth of the azeotropy rectification column of acetic acid recovery device body arranged evenly.
The present invention devises, and acetic acid recovery device body is set to also to include vapor preheater, cooler, phase-splitter, vapour coagulate water preheater, reboiler, entrainer tank and the pump housing,
The input port of spirit of vinegar is set to be communicated with and the input port that heated being set to coagulate with vapour water preheater by heating output port of vapor preheater is communicated with the input port that heated of vapor preheater, vapour coagulate water preheater be set to be communicated with the middle part input port of azeotropy rectification column by heating output port and the top input port of azeotropy rectification column is placed through the pump housing is communicated with the output port of entrainer tank, the top output port mouth of azeotropy rectification column is set to the heating input port connection of vapor preheater, the heating output port of vapor preheater is set to be communicated with the input port of cooler and the output port of cooler is set to be communicated with the input port of phase-splitter, the output port of phase-splitter is placed through the top input port of the pump housing and azeotropy rectification column respectively, the input port of entrainer tank is communicated with, the bottom output port of azeotropy rectification column is set to be communicated with the heating port of reboiler and the heating port being set to coagulate with vapour water preheater by heating port of reboiler is communicated with.
The present invention devises, and a kind of acetic acid recovery method based on azeotropic distillation, the steps include:
The middle part input port that spirit of vinegar coagulates from azeotropy rectification column after the preheating of water preheater two-stage through vapor preheater and vapour enters into azeotropy rectification column, entrainer enters into azeotropy rectification column by the top input port of azeotropy rectification column, discharge from the top output port mouth of azeotropy rectification column after water and entrainer mixing in azeotropy rectification column, phase-splitter is entered again after vapor preheater and cooler cooling, after static layering, water discharges process by bottom phase-splitter, entrainer is back to the top input port of azeotropy rectification column by the pump housing by the extraction of phase-splitter top, recycle, acetic acid is discharged with gas phase state at the tower bottom side of azeotropy rectification column.
The present invention devises, and entrainer is set to butyl acetate and with the 0.9-1:1 ratio of weight ratio according to entrainer and spirit of vinegar, entrainer is joined in spirit of vinegar.
The present invention devises, and rectifying column tower diameter is set to φ 900-1100, the number of plates is set to 70-74 and reflux ratio is set to 3-4.
Technique effect of the present invention is: the spirit of vinegar from front workshop section enters azeotropy rectification column after rectifying tower top steam and the preheating of steam-condensation water preheater two-stage in the middle part of rectifying column, improve into tower temperature after two-stage preheating, saved the consumption of steam.Entrainer is added by rectifying column tower top, steams with entrainer at Ta Zhongshui from tower top, after condenser cooling, enter phase-splitter, after static layering, water by bottom phase-splitter discharge process, entrainer by the extraction of phase-splitter top by pump reflux in rectifying column, recycle.At tower bottom side, gas phase extraction high concentration, the high-quality finished product acetic acid of rectifying column.Adopt azeotropic distillation, rectifying column tower diameter, the required number of plates and reflux ratio can be made to reduce, and energy consumption also can decrease.By this device, from tower spirit phase extraction acetic acid, concentration and the quality of acetic acid can be significantly improved.The concentration of acetic acid can be brought up to more than 95%.Improve the product competitiveness of enterprise, improve the competitive strength of enterprise.Employing adds entrainer recovery of acetic acid, can reduce tower diameter, reduces the number of plates, significantly reduces the investment of enterprise, reduces the carrying amount of acetic acid in overhead vapours simultaneously, improves the rate of recovery of acetic acid.Adopt overhead vapours and condensed water preheater preheats water-containing acetic acid, improve feeding temperature after two-stage preheating, reduce the consumption of steam, ton finished product can reduce steam consumption 0.5 ton, saves the production cost of enterprise.Adopt overhead water steam preheating material liquid, significantly can reduce the use amount of recirculated water, save recirculated water 10%.
In the technical program, the acetic acid recovery device body making the water in spirit of vinegar and entrainer be mixed to form the mixed liquor had a long way to go with acetic acid boiling point is important technical characteristic, in the technical field of the acetic acid recovery device and method based on azeotropic distillation, have novelty, creativeness and practicality, the term in the technical program is all to make an explanation with patent document in the art and to understand.
Four, accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the schematic diagram of background technology of the present invention:
Fig. 2 is schematic diagram of the present invention.
1-azeotropy rectification column, 2-vapor preheater, 3-cooler, 4-phase-splitter, 5-vapour coagulate water preheater, 6-reboiler, 7-entrainer tank, the 8-pump housing.
Five, detailed description of the invention
A kind of acetic acid recovery device based on azeotropic distillation, below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Fig. 1 is one embodiment of the present of invention, illustrates the present embodiment by reference to the accompanying drawings, includes azeotropy rectification column 1, vapor preheater 2, cooler 3, phase-splitter 4, vapour coagulates water preheater 5, reboiler 6, entrainer tank 7 and the pump housing 8,
The input port of spirit of vinegar is set to be communicated with and the input port that heated being set to coagulate with vapour water preheater 5 by heating output port of vapor preheater 2 is communicated with the input port that heated of vapor preheater 2, vapour coagulate water preheater 5 be set to be communicated with the middle part input port of azeotropy rectification column 1 by heating output port and the top input port of azeotropy rectification column 1 is placed through the pump housing 8 is communicated with the output port of entrainer tank 7, the top output port mouth of azeotropy rectification column 1 is set to the heating input port connection of vapor preheater 2, the heating output port of vapor preheater 2 is set to be communicated with the input port of cooler 3 and the output port of cooler 3 is set to be communicated with the input port of phase-splitter 4, the output port of phase-splitter 4 is placed through the top input port of the pump housing 8 and azeotropy rectification column 1 respectively, the input port of entrainer tank 7 is communicated with, the bottom output port of azeotropy rectification column 1 is set to be communicated with the heating port of reboiler 6 and the heating port being set to coagulate with vapour water preheater 5 by heating port of reboiler 6 is communicated with.
Based on an acetic acid recovery method for azeotropic distillation, below in conjunction with embodiment, further describe the present invention, following examples are intended to the present invention instead of limitation of the invention further are described.
First embodiment of the present invention, the steps include:
Spirit of vinegar coagulates after the preheating of water preheater 5 two-stage through vapor preheater 2 and vapour and enters into azeotropy rectification column 1 from the middle part input port of azeotropy rectification column 1, entrainer enters into azeotropy rectification column 1 by the top input port of azeotropy rectification column 1, discharge from the top output port mouth of azeotropy rectification column 1 after water and entrainer mixing in azeotropy rectification column 1, phase-splitter 4 is entered again after vapor preheater 2 and cooler 3 cool, after static layering, water discharges process by bottom phase-splitter 4, entrainer is back to the top input port of azeotropy rectification column 1 by the pump housing 8 by phase-splitter 4 top extraction, recycle, acetic acid is discharged with gas phase state at the tower bottom side of azeotropy rectification column 1.
In the present embodiment, entrainer is set to butyl acetate and with the 0.9:1 ratio of weight ratio according to entrainer and spirit of vinegar, entrainer is joined in spirit of vinegar.
In the present embodiment, rectifying column tower diameter be set to φ 1000, the number of plates be set to 72 and reflux ratio be set to 3.5.
For the acetic acid recovery device of daily output 30 tons, according to the existing method as Fig. 1, rectifying column tower diameter is φ 1600, the required number of plates be 85 and reflux ratio be 23-30, use the present embodiment, rectifying column tower diameter is φ 1000, the required number of plates be 72 and reflux ratio be 3.5, need vapours amount to save 30-40% simultaneously.
By the acetic acid that the method for such as Fig. 1 obtains, acetic acid color reaches national high-quality requirement, meets the requirement of numerous industry.Meanwhile, at the bottom of tower, acetic acid content reaches 95%, meets the requirements.
The technical essential of this enforcement is also: use butyl acetate as entrainer, by the combination of the parameter with rectifying column, best to the water treatment efficiency of spirit of vinegar, the parameter not only optimizing the miniaturization of rectifying column also improves the treatment effeciency of acetic acid.
Second embodiment of the present invention, entrainer is set to butyl acetate and with the 1:1 ratio of weight ratio according to entrainer and spirit of vinegar, entrainer is joined in spirit of vinegar.
Rectifying column tower diameter is set to φ 900, the number of plates be set to 70 and reflux ratio be set to 3.
3rd embodiment of the present invention, entrainer is set to butyl acetate and with the 0.95:1 ratio of weight ratio according to entrainer and spirit of vinegar, entrainer is joined in spirit of vinegar.
Rectifying column tower diameter is set to 1100, the number of plates be set to 74 and reflux ratio be set to 4.
4th embodiment of the present invention, entrainer is set to butyl acetate and with the 0.91:1 ratio of weight ratio according to entrainer and spirit of vinegar, entrainer is joined in spirit of vinegar.
Rectifying column tower diameter is set to φ 910, the number of plates be set to 73 and reflux ratio be set to 4.
Acetate butyl and butyl acetate are the colourless liquid having fruital smell.Butyl acetate is slightly soluble in water, can be miscible with the common organic solvents such as alcohol, ether.Butyl acetate is compared with lower homologue, and butyl acetate is insoluble in water, also more difficult hydrolysis.But under the effect of acid or alkali, hydrolysis generates acetic acid and butanols.
The present invention has lower feature:
1, owing to devising acetic acid recovery device body, by entering spirit of vinegar at azeotropy rectification column 1 pars intermedia, enter entrainer at the top of azeotropy rectification column 1, the water in spirit of vinegar and entrainer can be made to be mixed to form the mixed liquor had a long way to go with acetic acid boiling point, no longer directly enter spirit of vinegar from azeotropy rectification column 1 top, therefore optimize rectifying column tower diameter, the required number of plates and reflux ratio parameter, save vapours amount.
2, owing to devising vapor preheater 2, cooler 3, phase-splitter 4, vapour coagulates water preheater 5, reboiler 6, entrainer tank 7 and the pump housing 8, spirit of vinegar improves into azeotropy rectification column 1 temperature after two-stage preheating, has saved the consumption of steam.
3, owing to devising butyl acetate, the mixed liquor be mixed to form by the water in spirit of vinegar and butyl acetate.
4, owing to devising, the restriction of number range has been carried out to planform, number range is made to be technical characteristic in technical scheme of the present invention, be not by formulae discovery or tested the technical characteristic drawn by limited number of time, test shows that the technical characteristic of this number range achieves good technique effect.
5, owing to devising technical characteristic of the present invention, in the effect of the set separately and each other of technical characteristic, by test show, property indices of the present invention be existing property indices be at least 1.7 times, by assessment there is good market value.
Other technical characteristic connected with the acetic acid recovery device body that the water made in spirit of vinegar and entrainer are mixed to form the mixed liquor had a long way to go with acetic acid boiling point also having other is all one of embodiments of the invention, and each technical characteristic of the above embodiment can combine arbitrarily, for meeting the requirement of Patent Law, patent regulation and guidelines for examination, no longer the embodiment of all possible combination of each technical characteristic in above-described embodiment is all described.
Therefore based in the acetic acid recovery device and method technical field of azeotropic distillation; everyly include the acetic acid recovery device body with azeotropy rectification column 1, the pars intermedia of azeotropy rectification column 1 be provided with spirit of vinegar input port, be provided with at the top of azeotropy rectification column 1 entrainer input port and be provided with the technology contents of the output port of acetic acid all in protection scope of the present invention at the tower bottom side of azeotropy rectification column 1 face.
Above-described embodiment is a kind of way of realization of the acetic acid recovery device and method based on azeotropic distillation provided by the present invention; according to other distortion of scheme provided by the present invention; the composition increased or reduce wherein or step; or the present invention is used for other the technical field close with the present invention, all belongs to protection scope of the present invention.
Claims (6)
1. the acetic acid recovery device based on azeotropic distillation, it is characterized in that: include the acetic acid recovery device body with azeotropy rectification column (1), the pars intermedia of azeotropy rectification column (1) be provided with spirit of vinegar input port, be provided with at the top of azeotropy rectification column (1) entrainer input port and the tower bottom side of azeotropy rectification column (1) face is provided with the output port of acetic acid.
2. the acetic acid recovery device based on azeotropic distillation according to claim 1, is characterized in that: the mode being mixed to form the mixed liquor had a long way to go with acetic acid boiling point according to the water made in spirit of vinegar and entrainer is carried out the material input mouth of the azeotropy rectification column of acetic acid recovery device body (1) arranged evenly.
3. the acetic acid recovery device based on azeotropic distillation according to claim 1, it is characterized in that: acetic acid recovery device body is set to also include vapor preheater (2), cooler (3), phase-splitter (4), vapour coagulates water preheater (5), reboiler (6), entrainer tank (7) and the pump housing (8), the input port of spirit of vinegar is set to be communicated with and the input port that heated being set to coagulate with vapour water preheater (5) by heating output port of vapor preheater (2) is communicated with the input port that heated of vapor preheater (2), vapour coagulate water preheater (5) be set to be communicated with the middle part input port of azeotropy rectification column (1) by heating output port and the top input port of azeotropy rectification column (1) is placed through the pump housing (8) is communicated with the output port of entrainer tank (7), the top output port mouth of azeotropy rectification column (1) is set to the heating input port connection of vapor preheater (2), the heating output port of vapor preheater (2) is set to be communicated with the input port of cooler (3) and the output port of cooler (3) is set to be communicated with the input port of phase-splitter (4), the output port of phase-splitter (4) is placed through the top input port of the pump housing (8) and azeotropy rectification column (1) respectively, the input port of entrainer tank (7) is communicated with, the bottom output port of azeotropy rectification column (1) is set to be communicated with the heating port of reboiler (6) and the heating port being set to coagulate with vapour water preheater (5) by heating port of reboiler (6) is communicated with.
4. a kind of acetic acid recovery method based on azeotropic distillation of the acetic acid recovery device based on azeotropic distillation according to claim 1, is characterized in that: the steps include:
Spirit of vinegar coagulates after water preheater (5) two-stage preheating through vapor preheater (2) and vapour and enters into azeotropy rectification column (1) from the middle part input port of azeotropy rectification column (1), entrainer enters into azeotropy rectification column (1) by the top input port of azeotropy rectification column (1), discharge from the top output port mouth of azeotropy rectification column (1) after water and entrainer mixing in azeotropy rectification column (1), phase-splitter (4) is entered again after vapor preheater (2) and cooler (3) cooling, after static layering, water discharges process by phase-splitter (4) bottom, entrainer is back to the top input port of azeotropy rectification column (1) by the pump housing (8) by phase-splitter (4) top extraction, recycle, acetic acid is discharged with gas phase state at the tower bottom side of azeotropy rectification column (1).
5. the acetic acid recovery method based on azeotropic distillation according to claim 4, is characterized in that: entrainer is set to butyl acetate and with the 0.9-1:1 ratio of weight ratio according to entrainer and spirit of vinegar, entrainer is joined in spirit of vinegar.
6. the acetic acid recovery method based on azeotropic distillation according to claim 4, is characterized in that: rectifying column tower diameter is set to φ 900-1100, the number of plates is set to 70-74 and reflux ratio is set to 3-4.
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| CN201510820644.XA CN105381624A (en) | 2015-11-24 | 2015-11-24 | Azeotropy rectification method-based acetic acid recovery device and method |
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| CN201510820644.XA CN105381624A (en) | 2015-11-24 | 2015-11-24 | Azeotropy rectification method-based acetic acid recovery device and method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107617227A (en) * | 2017-10-30 | 2018-01-23 | 广西万山香料有限责任公司 | The process units of trans-anethole rectifying section |
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| CN107617227B (en) * | 2017-10-30 | 2023-12-15 | 广西玉蓝生物科技有限公司 | Production device of anethole rectifying section |
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