CN103641680B - The method and apparatus of two extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution - Google Patents
The method and apparatus of two extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution Download PDFInfo
- Publication number
- CN103641680B CN103641680B CN201310694873.2A CN201310694873A CN103641680B CN 103641680 B CN103641680 B CN 103641680B CN 201310694873 A CN201310694873 A CN 201310694873A CN 103641680 B CN103641680 B CN 103641680B
- Authority
- CN
- China
- Prior art keywords
- tower
- ethanol
- benzene
- mixed solution
- integration device
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- C07C29/84—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation
-
- 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
- B01D3/40—Extractive distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The method and apparatus of two extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution.The mixed solution of ritalin, methyl alcohol, ethanol, benzene and water is separated through two extracting rectifying discharging tower integration device: the middle and lower part of raw material access to plant side; Side tower top temperature controls, at 55.5 ~ 56.8 DEG C, to obtain the mixed solution of the ritalin of more than 99.8%, methyl alcohol, ethanol and benzene; Opposite side tower top temperature is 64.1 ~ 65.5 DEG C, and top obtains higher than 99% methanol solution; Tower reactor flows out containing the mixed solution of extraction agent through regenerator column process, and regenerator column tower top can more than 48% ethanolic soln; Extraction agent at the bottom of tower is circulated to device both sides and recycles.Present invention process step is simple, yield is high, and energy consumption is low.After treatment, once can obtain the azeotrope of the ritalin of more than 99.8%, methyl alcohol, ethanol and benzene, yield can reach more than 95% to stock liquid, obtains more than 99% methyl alcohol at partition opposite side simultaneously.
Description
Technical field
The present invention relates to the extraction integrated technique that multicomponent mixture is separated, be specifically related to the method for a kind of pair of extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution.The invention still further relates to the equipment that this method uses.
Background technology
Ritalin, methyl alcohol, ethanol and benzene are important industrial chemicals and solvent, extensive pharmacy and pesticide intermediate synthetic, in pharmacy and pesticide intermediate building-up process, adopt above-mentioned solvent, the mixing solutions of easy formation ritalin, methyl alcohol, ethanol, benzene and water, in above-mentioned mixing solutions, ritalin, ethanol, methyl alcohol, benzene and water form binary, ternary azeotrope each other, adopt conventional distillation method to be separated.Traditional industry adopts the accurate azeotropic distillation that adds water to extract ritalin, methyl alcohol, the mixture of ethanol and benzene, then precise distillation is adopted to extract methyl alcohol and ethanol, adopt aforesaid method can obtain content about 99% ritalin, methyl alcohol, the azeotrope of ethanol and benzene, then methyl alcohol and the ethanol of about 99% is obtained respectively by precise distillation method, but this process is more complicated, ritalin, methyl alcohol, a yield of ethanol and benzene is all lower than 47%, need through separating for several times, separation yield could be improved, azeotropic distillation and precise distillation process reflux ratio are all higher than 8:1, process energy consumption is high.
Summary of the invention
The present invention by provide a kind of pair of extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution method and apparatus, compared with traditional technology, novel method processing step is fairly simple, yield is high, and extraction agent is convenient to reclaim, recycle, energy consumption is low.The present invention adopts two extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution, stock liquid is after the process of two extracting rectifying unification tower, once can obtain the azeotrope of the ritalin of more than 99.8%, methyl alcohol, ethanol and benzene, yield can reach more than 95%, obtain more than 99% methyl alcohol at partition opposite side simultaneously, this technological process is simple, and energy consumption is low.
The technical scheme completing foregoing invention task is, the method of a kind of pair of extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene 2-water mixed solution, the mixed solution of ritalin, methyl alcohol, ethanol, benzene and water is separated through two extracting rectifying discharging tower integration device, and it is characterized in that, step is as follows:
(1). the mixed solution of ritalin, methyl alcohol, ethanol, benzene and water enters the middle and lower part of two extracting rectifying discharging tower integration device side;
(2). side tower top temperature controls, at 55.5 ~ 56.8 DEG C, to obtain the mixed solution of the ritalin of mass ratio more than 99.8%, methyl alcohol, ethanol and benzene, and the mass content of water is lower than 0.2%;
(3). simultaneously at the opposite side of two extracting rectifying discharging tower integration device, tower top temperature is 64.1 ~ 65.5 DEG C, and top obtains mass ratio higher than 99% methanol solution;
(4). tower reactor outflow contains the mixed solution of extraction agent through regenerator column process, and regenerator column tower top can obtain mass ratio more than 48% ethanolic soln;
(5). extraction agent at the bottom of regenerator column tower is circulated to the both sides of two extracting rectifying discharging tower integration device, recycles.
In prioritization scheme, step (2) with step (3) in, two extractive distillation column sides trim the top of column adopt external reflux, opposite side adopt internal reflux.
Specifically, present method step is as follows: ritalin, methyl alcohol, ethanol, 1. the mixed solution of benzene and water enters the middle and lower part of two extracting rectifying discharging tower integration device side, tower top side and opposite side temperature are respectively 55.5 ~ 56.8 DEG C and 64.1 ~ 65.5 DEG C, extraction agent (90-95% glycerol and 5-10% Potassium ethanoate) is 2. with 7. respectively in the both sides upper position charging of two extracting rectifying discharging tower integration device, both sides solvent equal proportion charging, 3. tower top is 99.8% ritalin, methyl alcohol, the mixed solution of ethanol and benzene, 4. the opposite side top of two extracting rectifying discharging tower integration device obtain higher than 99% methanol solution, 5. the bottom of device is the mixed solution containing extraction agent, tower reactor mixed solution is through regenerator column process, and regeneration overhead distillates the ethanolic soln that 6. cut is more than 48% respectively, and extraction agent at the bottom of regenerator column tower is circulated to the both sides of two extracting rectifying discharging tower integration device, recycles.The processing condition of sepn process: in sepn process, each bottom temperature control, reflux ratio, feed entrance point and stage number are shown in Table 1.
Table 1 sepn process processing condition
Table 1 sepn process processing condition
The technical scheme completing the application's second invention task is: the equipment that the method for above-mentioned pair of extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution uses, it is characterized in that, be provided with two extracting rectifying discharging tower integration device, the middle and lower part of this pair of extracting rectifying discharging tower integration device side is provided with material inlet; The centre of this pair of extracting rectifying discharging tower integration device, is provided with longitudinal partition, and described pair of extracting rectifying discharging tower integration device is divided into left and right two portions by this partition; Well heater is equipped with at the bottom of the described pair of two-part tower in extracting rectifying discharging tower integration device left and right; Backflow side line drawing mechanism is respectively equipped with in the described pair of two-part tower top in extracting rectifying discharging tower integration device left and right; Be connected with regenerator column by pipeline at the bottom of the tower of this pair of extracting rectifying discharging tower integration device.
In the prioritization scheme of above equipment:
Be connected with the both sides of two extracting rectifying discharging tower integration device respectively by pipeline at the bottom of the tower of regenerator column, extraction agent at the bottom of tower be circulated to the both sides of two extracting rectifying discharging tower integration device, recycle;
All filler is filled with in described pair of extracting rectifying discharging tower integration device left and right two portions;
Described regenerator column inside is also provided with filler.
Compared with traditional technology, present invention process step is fairly simple, yield is high, and extraction agent is convenient to reclaim, and recycle, energy consumption is low.Central Plains of the present invention feed liquid is after the process of two extracting rectifying unification tower, and once can obtain the azeotrope of the ritalin of more than 99.8%, methyl alcohol, ethanol and benzene, yield can reach more than 95%, obtains more than 99% methyl alcohol at partition opposite side simultaneously.
Accompanying drawing explanation
Fig. 1 is two extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution device structure schematic diagram.
Embodiment
Two extractive distillation column unification tripping device reference Fig. 1, two extracting rectifying discharging tower integration device 1, the middle and lower part of its side is provided with material inlet; The centre of this pair of extracting rectifying discharging tower integration device 1, is provided with longitudinal partition 6, and described pair of extracting rectifying discharging tower integration device is divided into left and right two portions by this partition 6; Well heater 3,9 is equipped with at the bottom of the described pair of two-part tower in extracting rectifying discharging tower integration device left and right; Backflow side line drawing mechanism 4 is respectively equipped with in the described pair of two-part tower top in extracting rectifying discharging tower integration device left and right; Be connected with regenerator column 7 by pipeline at the bottom of the tower of this pair of extracting rectifying discharging tower integration device 1.Methyl acetate and methanol-ethanol-benzene-the water mixed liquid adopting associated companies to provide is raw material, two extracting rectifying discharging tower integration device experiment is carried out at ambient pressure, tower internal diameter is 50mm, tower diameter separates by equal proportion by partition, the Stainless Steel Helices of in-built φ 3*3 θ type, through measuring by standards system, this height equivalent to one theoretical plate HETP=27mm, tower reactor electric mantle heats, overhead product discharging and raw material, solvent feed and discharging are all measured with glass rotameter, two extractive distillation column sides trim the top of column adopts external reflux, and opposite side adopts internal reflux.Raw material ritalin, methyl alcohol, ethanol, 1. the mixed solution of benzene and water enters the middle and lower part of two extracting rectifying discharging tower integration device side, tower top side and opposite side temperature are respectively 55.5 ~ 56.8 DEG C and 41.3 ~ 52.9 DEG C, extraction agent (90-95% glycerol and 5-10% Potassium ethanoate) is 2. with 7. respectively in the both sides upper position charging of two extracting rectifying discharging tower integration device, both sides solvent equal proportion charging, 3. tower top is 99.8% ritalin, methyl alcohol, the mixed solution of ethanol and benzene, 4. the opposite side top of two extracting rectifying discharging tower integration device obtain higher than 99% methanol solution, 5. the bottom of device is the mixed solution containing extraction agent, tower reactor mixed solution is through regenerator column process, and regenerator column operates at reduced pressure conditions, and regeneration overhead distillates the ethanolic soln that 6. cut is more than 48%, and extraction agent at the bottom of regenerator column tower is circulated to the both sides of two extracting rectifying discharging tower integration device, recycles.Analyze through HP chromatographic instrument, raw material and each fractions consisting detailed results are shown in Table 2.
Table 2 pair extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution separating resulting
Claims (3)
1. a method for two extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution, the mixed solution of ritalin, methyl alcohol, ethanol, benzene and water is separated through two extracting rectifying discharging tower integration device, and it is characterized in that, step is as follows:
(1). the mixed solution of ritalin, methyl alcohol, ethanol, benzene and water enters the middle and lower part of two extracting rectifying discharging tower integration device side;
Extraction agent respectively in the both sides upper position charging of two extracting rectifying discharging tower integration device, both sides solvent equal proportion charging;
(2). side tower top temperature controls, at 55.5 ~ 56.8 DEG C, to obtain the mixed solution of the ritalin of mass ratio more than 99.8%, methyl alcohol, ethanol and benzene, and the mass content of water is lower than 0.2%;
. simultaneously at the opposite side of two extracting rectifying discharging tower integration device, tower top temperature is 64.1 ~ 65.5 DEG C, top obtain mass ratio higher than 99% methanol solution;
(4). tower reactor outflow contains the mixed solution of extraction agent through regenerator column process, and regenerator column tower top can obtain the ethanolic soln of mass ratio more than 48%;
(5). extraction agent at the bottom of regenerator column tower is circulated to the both sides of two extracting rectifying discharging tower integration device, recycles;
The middle and lower part of described pair of extracting rectifying discharging tower integration device side is provided with material inlet; The centre of this pair of extracting rectifying discharging tower integration device, is provided with longitudinal partition, and described pair of extracting rectifying discharging tower integration device is divided into left and right two portions by this partition; Well heater is equipped with at the bottom of the described pair of two-part tower in extracting rectifying discharging tower integration device left and right; Backflow side line drawing mechanism is respectively equipped with in the described pair of two-part tower top in extracting rectifying discharging tower integration device left and right; Be connected with regenerator column by pipeline at the bottom of the tower of this pair of extracting rectifying discharging tower integration device.
2. the method for according to claim 1 pair of extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution, it is characterized in that, step (2) with step (3) in, two extractive distillation column sides trim the top of column adopt external reflux, opposite side adopt internal reflux.
3. the method for according to claim 1 pair of extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution, it is characterized in that, processing parameter is as table 1:
Table 1 sepn process processing condition
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310694873.2A CN103641680B (en) | 2013-12-17 | 2013-12-17 | The method and apparatus of two extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310694873.2A CN103641680B (en) | 2013-12-17 | 2013-12-17 | The method and apparatus of two extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103641680A CN103641680A (en) | 2014-03-19 |
| CN103641680B true CN103641680B (en) | 2015-12-30 |
Family
ID=50247013
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310694873.2A Active CN103641680B (en) | 2013-12-17 | 2013-12-17 | The method and apparatus of two extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103641680B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116082159B (en) * | 2022-12-22 | 2024-06-04 | 重庆科技学院 | Method for separating ethyl acetate-methanol-water by coupling heterogeneous phase and three-tower rectification |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102159291A (en) * | 2008-09-17 | 2011-08-17 | 巴斯夫欧洲公司 | Devices and method for continuous distillative separation of mixture containing one or more alkanolamine(s) |
| CN102190559A (en) * | 2011-03-25 | 2011-09-21 | 浙江大学 | Method and device for refining methanol by using divided wall distillation column |
| EP2409746A2 (en) * | 2009-03-19 | 2012-01-25 | LG Chem, Ltd. | Dividing wall distillation columns for production of high-purity 2-ethylhexanol and fractionation method using same |
-
2013
- 2013-12-17 CN CN201310694873.2A patent/CN103641680B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102159291A (en) * | 2008-09-17 | 2011-08-17 | 巴斯夫欧洲公司 | Devices and method for continuous distillative separation of mixture containing one or more alkanolamine(s) |
| EP2409746A2 (en) * | 2009-03-19 | 2012-01-25 | LG Chem, Ltd. | Dividing wall distillation columns for production of high-purity 2-ethylhexanol and fractionation method using same |
| CN102190559A (en) * | 2011-03-25 | 2011-09-21 | 浙江大学 | Method and device for refining methanol by using divided wall distillation column |
Non-Patent Citations (1)
| Title |
|---|
| Dividing wall columns in chemical process industry: A review on current activities;Ömer Yildirim，et al.;《Separation and Purification Technology》;20110526;第80卷;403-417 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103641680A (en) | 2014-03-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP2947065B1 (en) | Device and process for preparing an octanol | |
| CN103435482B (en) | Separation method and separation device of synthesis gas ethylene glycol product | |
| CN102718826B (en) | Method for extracting and separating 24-dehydrocholesterol and cholesterol by ionic liquid | |
| CN103664446A (en) | Technology for separating n-hexane-methylcyclopentane through extractive distillation | |
| CN105348035A (en) | Method for integrated purification of chloroform and ethyl acetate mixed solution through azeotropic extractive distillation and liquid-liquid delamination | |
| CN102633597B (en) | Process of recovering ethanol, propyl alcohol and isobutyl alcohol from polyalcohol-water mixture | |
| CN103641680B (en) | The method and apparatus of two extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution | |
| CN106478370A (en) | A kind of method for reclaiming methyl alcohol in improved methanol rectification periodic off-gases | |
| CN101898963A (en) | Method for separating methyl acetate-methanol-water by adopting extractive distillation separation method with two-solvent lateral feed | |
| CN100575332C (en) | The method of salting, compounding, extracting, rectifying separating ethyl acetate-ethanol-water mixed liquid | |
| CN103755522B (en) | A kind of ion liquid abstraction rectification separation methanol--device of methyl acetate | |
| CN105924350A (en) | Processing method for producing dimethyl carbonate byproduct pharmaceutical grade propylene glycol through transesterification method | |
| CN103752030A (en) | Ionic liquid extractive distillation experiment device | |
| CN103833537B (en) | Absorption and refining method for high-purity methylacrolein | |
| CN105949026A (en) | Mixed pentane precise separation device | |
| CN104693005A (en) | New process for separating methanol-propyl formate azeotrope through extractive distillation | |
| CN203677981U (en) | Ionic liquid extractive distillation experimental device | |
| CN102432462B (en) | Method for extracting, rectifying and separating methylene dichloride, ethanol and ethyl acetate | |
| CN103910629A (en) | Method used for smooth and steady preparation of 2-methoxypropandioic acid ethyl methyl ester | |
| CN103193590A (en) | Method for continuously extracting, rectifying and separating mixed alcohols from water | |
| CN1226261C (en) | Liquid-liquid extraction process of dioxyethyl methane and water solution of ethanol | |
| CN100551891C (en) | Combine with the chromatography method of extraction of high purity solanesol alcohol of multi-stage solvent extraction crystallization | |
| CN106831336B (en) | Ethyl alcohol and the recycling of hydrazine hydrate mixed liquor and circulation utilization method in a kind of production of pyraclostrobin | |
| CN105906488B (en) | A kind of purification purifying plant for by-product diisopropyl ether in isopropyl alcohol production | |
| CN101780114A (en) | Extraction and separation method of effective constituents of traditional Chinese medicine |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |