CN103641680A - Method and equipment for combined separation of methyl acetate-methanol-ethanol-benzene-water mixed solution employing double extraction rectification tower - Google Patents
Method and equipment for combined separation of methyl acetate-methanol-ethanol-benzene-water mixed solution employing double extraction rectification tower Download PDFInfo
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- CN103641680A CN103641680A CN201310694873.2A CN201310694873A CN103641680A CN 103641680 A CN103641680 A CN 103641680A CN 201310694873 A CN201310694873 A CN 201310694873A CN 103641680 A CN103641680 A CN 103641680A
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- 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
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Abstract
The invention discloses a method and equipment for combined separation of a methyl acetate-methanol-ethanol-benzene-water mixed solution employing a double extraction rectification tower. The methyl acetate-methanol-ethanol-benzene-water mixed solution is separated by a combined separation device of the double extraction rectification tower; raw materials enter the middle and lower part at one side of the device; the tower top temperature at one side is controlled at 55.5-56.8 DEG C, so as to obtain over 99.8% of mixed solution of methyl acetate, methanol, ethanol and benzene; the tower top temperature at the other side is 64.1-65.5 DEG C; over 99% of methanol solution is obtained at the upper part; the mixed solution containing an extraction agent flowing from the tower is processed by a regeneration tower; over 48% of ethanol solution can be obtained from the top of the regeneration tower; and the extraction agent at the bottom of the tower is circulated to two sides to be recycled. The technology disclosed by the invention is simple in steps, high in yield and low in energy consumption, over 99.8% of azeotrope of methyl acetate, methanol, ethanol and benzene can be obtained from a raw material solution one time after treatment, the yield can be up to over 95%, and meanwhile, over 99% of methanol is obtained at the other side of a dividing wall.
Description
Technical field
The present invention relates to the extraction integrated technique of multicomponent mixture separation, 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 is used.
Background technology
Ritalin, methyl alcohol, ethanol and benzene are important industrial chemicals and solvents, extensive pharmacy and pesticide intermediate synthetic, in pharmacy and pesticide intermediate building-up process, adopt above-mentioned solvent, easily form the mixing solutions of 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, and employing conventional distillation method cannot be separated.Traditional industry adopts and adds the close azeotropic distillation extraction of crystal ritalin, methyl alcohol, the mixture of ethanol and benzene, then adopt precise distillation to extract methyl alcohol and ethanol, adopt aforesaid method can obtain content 99% left and right ritalin, methyl alcohol, the azeotrope of ethanol and benzene, then by precise distillation method, obtain respectively methyl alcohol and the ethanol of 99% left and right, 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, could improve separation yield, 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, compare 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 solutions, stock liquid is after two extracting rectifying unification towers are processed, can once obtain the azeotrope of more than 99.8% ritalin, methyl alcohol, ethanol and benzene, yield can reach more than 95%, at partition opposite side, obtain 99% above methyl alcohol simultaneously, this technological process is simple, and energy consumption is low.
The technical scheme that completes foregoing invention task is, the method of a kind of pair of 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 devices, 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 one sides;
(2). a side tower top temperature is controlled at 55.5～56.8 ℃, obtains the mixed solution of more than 99.8% ritalin, methyl alcohol, ethanol and the benzene of mass ratio, and the mass content of water is lower than 0.2%;
(3). at the opposite side of two extracting rectifying discharging tower integration devices, tower top temperature is 64.1～65.5 ℃ simultaneously, and top obtains mass ratio higher than 99% methanol solution;
(4). tower reactor flows out containing the mixed solution of extraction agent to be processed through regenerator column, and regenerator column tower top can obtain the above ethanolic soln of mass ratio 48%;
(5). at the bottom of regenerator column tower, extraction agent is circulated to the both sides of two extracting rectifying discharging tower integration devices, recycles.
In prioritization scheme, step (2) with step (3) in, two extractive distillation column one side trim the top of column adopt external refluxs, opposite side adopts 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 one sides, tower top one side and opposite side temperature are respectively 55.5～56.8 ℃ and 64.1～65.5 ℃, extraction agent (90-95% glycerol and 5-10% Potassium ethanoate) is 2. with 7. respectively in the upper position charging of the both sides of two extracting rectifying discharging tower integration devices, 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 devices obtain higher than 99% methanol solution, 5. the bottom of device is the mixed solution containing extraction agent, tower reactor mixed solution is processed through regenerator column, and 6. regeneration overhead distillates respectively cut is more than 48% ethanolic soln, and at the bottom of regenerator column tower, extraction agent is circulated to the both sides of two extracting rectifying discharging tower integration devices, recycles.The processing condition of sepn process: in sepn process, each tower reactor temperature control, reflux ratio, feed entrance point and stage number are shown in Table 1.
Table 1 sepn process processing condition
The technical scheme that completes second invention task of the application 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 is used, it is characterized in that, be provided with two extracting rectifying discharging tower integration devices, the middle and lower part of this pair of extracting rectifying discharging tower integration device one side is provided with material inlet; The centre of this pair of extracting rectifying discharging tower integration device, is provided with partition longitudinally, and this partition is divided into left and right two portions by described pair of extracting rectifying discharging tower integration device; At the bottom of the described pair of two-part tower in extracting rectifying discharging tower integration device left and right, be equipped with well heater; In the described pair of two-part tower top in extracting rectifying discharging tower integration device left and right, be respectively equipped with backflow side line drawing mechanism; At the bottom of the tower of this pair of extracting rectifying discharging tower integration device, by pipeline, be connected with regenerator column.
In the prioritization scheme of above equipment:
At the bottom of the tower of regenerator column, by pipeline, be connected with the both sides of two extracting rectifying discharging tower integration devices respectively, extraction agent at the bottom of tower be circulated to the both sides of two extracting rectifying discharging tower integration devices, recycle;
In described pair of extracting rectifying discharging tower integration device left and right two portions, be all filled with filler;
Described regenerator column inside is also provided with filler.
Compare with traditional technology, processing step of the present invention is fairly simple, yield is high, and extraction agent is convenient to reclaim, recycle, and energy consumption is low.Central Plains of the present invention feed liquid, after two extracting rectifying unification towers are processed, can once obtain the azeotrope of more than 99.8% ritalin, methyl alcohol, ethanol and benzene, and yield can reach more than 95%, at partition opposite side, obtains 99% above methyl alcohol 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 columns are unified tripping devices with reference to Fig. 1, two extracting rectifying discharging tower integration devices 1, and the middle and lower part of one side is provided with material inlet; The centre of this pair of extracting rectifying discharging tower integration device 1, is provided with partition 6 longitudinally, and this partition 6 is divided into left and right two portions by described pair of extracting rectifying discharging tower integration device; At the bottom of the described pair of two-part tower in extracting rectifying discharging tower integration device left and right, be equipped with well heater 3,9; In the described pair of two-part tower top in extracting rectifying discharging tower integration device left and right, be respectively equipped with backflow side line drawing mechanism 4; At the bottom of the tower of this pair of extracting rectifying discharging tower integration device 1, by pipeline, be connected with regenerator column 7.Methyl acetate and methanol-ethanol-benzene-the water mixed liquid that adopts associated companies to provide is raw material, two extracting rectifying discharging tower integration device experiments are carried out under normal pressure, tower internal diameter is 50mm, partition separates tower diameter by equal proportion, 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 heats with electric mantle, overhead product discharging and raw material, solvent feed and discharging are all measured with glass rotameter, two extractive distillation column one side trim the top of column adopt 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 one sides, tower top one side and opposite side temperature are respectively 55.5～56.8 ℃ and 41.3～52.9 ℃, extraction agent (90-95% glycerol and 5-10% Potassium ethanoate) is 2. with 7. respectively in the upper position charging of the both sides of two extracting rectifying discharging tower integration devices, 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 devices obtain higher than 99% methanol solution, 5. the bottom of device is the mixed solution containing extraction agent, tower reactor mixed solution is processed through regenerator column, and regenerator column operates under reduced pressure, and 6. regeneration overhead distillates cut is more than 48% ethanolic soln, and at the bottom of regenerator column tower, extraction agent is circulated to the both sides of two extracting rectifying discharging tower integration devices, recycles.Through HP chromatographic instrument, analyze, 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 (9)
1. two extractive distillation columns are unified a method for separating methyl acetate and methanol-ethanol-benzene-water mixed solutions, and the mixed solution of ritalin, methyl alcohol, ethanol, benzene and water is separated through two extracting rectifying discharging tower integration devices, 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 one sides;
(2). a side tower top temperature is controlled at 55.5～56.8 ℃, obtains the mixed solution of more than 99.8% ritalin, methyl alcohol, ethanol and the benzene of mass ratio, and the mass content of water is lower than 0.2%;
(3). at the opposite side of two extracting rectifying discharging tower integration devices, tower top temperature is 64.1～65.5 ℃ simultaneously, and top obtains mass ratio higher than 99% methanol solution;
(4). tower reactor flows out containing the mixed solution of extraction agent to be processed through regenerator column, and regenerator column tower top can obtain the above ethanolic soln of mass ratio 48%;
(5). at the bottom of regenerator column tower, extraction agent is circulated to the both sides of two extracting rectifying discharging tower integration devices, recycles.
In prioritization scheme, step (2) with step (3) in, two extractive distillation column one side trim the top of column adopt external refluxs, opposite side adopts internal reflux.
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 one side trim the top of column adopt external refluxs, opposite side adopts 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, is characterized in that, processing parameter is as table 1:
Table 1 sepn process processing condition
4. the equipment that the method for two extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solutions of claim 1 is used, it is characterized in that, be provided with two extracting rectifying discharging tower integration devices, the middle and lower part of this pair of extracting rectifying discharging tower integration device one side is provided with material inlet; The centre of this pair of extracting rectifying discharging tower integration device, is provided with partition longitudinally, and this partition is divided into left and right two portions by described pair of extracting rectifying discharging tower integration device; At the bottom of the described pair of two-part tower in extracting rectifying discharging tower integration device left and right, be equipped with well heater; In the described pair of two-part tower top in extracting rectifying discharging tower integration device left and right, be respectively equipped with backflow side line drawing mechanism; At the bottom of the tower of this pair of extracting rectifying discharging tower integration device, by pipeline, be connected with regenerator column.
5. the equipment that the method for according to claim 4 pair of extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution is used, it is characterized in that, at the bottom of the tower of described regenerator column, by pipeline, be connected with the both sides of two extracting rectifying discharging tower integration devices respectively, the both sides that extraction agent at the bottom of tower are circulated to two extracting rectifying discharging tower integration devices, recycle.
6. the equipment that the method for according to claim 4 pair of extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution is used, is characterized in that, in described pair of extracting rectifying discharging tower integration device left and right two portions, is all filled with filler.
7. the equipment that the method for according to claim 4 pair of extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution is used, is characterized in that, described regenerator column inside is provided with filler.
8. the equipment that the method for according to claim 4 pair of extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solution is used, it is characterized in that, described partition is longitudinally that Jiang Shuan extracting rectifying discharging tower integration device separates tower diameter by equal proportion.
9. the equipment using according to the method for the two extractive distillation column unification separating methyl acetate and methanol-ethanol-benzene-water mixed solutions one of claim 4-8 Suo Shu, it is characterized in that the Stainless Steel Helices of the described pair of in-built φ 3*3 of extracting rectifying discharging tower integration device left and right two portions θ type; This height equivalent to one theoretical plate HETP=27mm.
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| CN116082159A (en) * | 2022-12-22 | 2023-05-09 | 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 |
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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 |
|---|
| ÖMER YILDIRIM，ET AL.: "Dividing wall columns in chemical process industry: A review on current activities", 《SEPARATION AND PURIFICATION TECHNOLOGY》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116082159A (en) * | 2022-12-22 | 2023-05-09 | 重庆科技学院 | Method for separating ethyl acetate-methanol-water by coupling heterogeneous phase and three-tower rectification |
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