CN102188832B - Separation column body for reaction distillation - Google Patents
Separation column body for reaction distillation Download PDFInfo
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- CN102188832B CN102188832B CN201010116328.1A CN201010116328A CN102188832B CN 102188832 B CN102188832 B CN 102188832B CN 201010116328 A CN201010116328 A CN 201010116328A CN 102188832 B CN102188832 B CN 102188832B
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Abstract
The invention relates to a separation column body for reaction distillation. The separation column body is mainly used for solving the problems that two columns (a reaction distillation column and a product partition column) are necessary for realization of the traditional reaction distillation process, and the procedure is complicated. In order to preferably solve the problems, the technical scheme is as follows: the separation column body comprises a material feed inlet, a column-top feed inlet, a column-top feed outlet, a column-bottom feed inlet, a column-bottom feed outlet, a side-line extraction feed outlet, division boards, a common rectifying section, a reaction section, an extraction-side rectifying section and a common stripping section, wherein the feed side can be provided with a rectifying section and/or a stripping section; the separation column body for the reaction distillation is divided into the common rectifying section, a feed-side rectifying section, the reaction section, a feed-side stripping section, the extraction-side rectifying section and the common stripping section by the division boards; in the section of reaction and distillation, the reaction section is located between the feed-side rectifying section and the feed-side stripping section, the feed-side rectifying section is located above the reaction section, and the feed-side stripping section is located below the reaction section; and the area between the tops of the division boards and the column-top feed inlet and the column-top feed outlet is the common rectifying section, the area between the bottoms of the division boards and the column-bottom feed inlet and the column-bottom feed outlet is the common stripping section, the other side of the material feed inlet in the area at which the division boards are located is the extraction-side rectifying section. The separation column body can be applied to industrial application for reaction distillation.
Description
Technical field
The present invention relates to a kind of reaction distillation and separate tower tower body.
Background technology
Catalytic distillation technology is that reaction is carried out in same catalysis-distillation equipment with separation of products, when reaction is carried out, the separation of products generating is gone out, and the balance of reaction is broken, thereby makes reaction trend completely, improves the conversion ratio of reactant; Reaction heat can be absorbed by the vaporization of reaction mass in addition, thereby reaction temperature can keep constant, and energy consumption can greatly reduce, and technological process is simplified, and investment also greatly reduces.Catalytic distillation tower generally forms by three sections: top is rectifying section (not high to the quality requirement of overhead product or can not establish rectifying section while not requiring), and middle part is catalyst reaction section, and bottom is stripping section.In catalytic distillation tower, the liquid phase material flowing downward must also react and product fractionation by middle part catalyst reaction section therein with the mobile vapor-phase material that makes progress simultaneously in convection current.Chinese patent literature CN1380273A has introduced current methyl acetate catalysis rectification hydrolysis technique, and this technique is mainly comprised of catalytic rectifying tower, extractive distillation column, dealcoholize column, degreasing tower and azeotropy rectification column, and catalytic distillation is realized in different towers from product separation.At present common catalytic distillation technology flow chart is shown in Fig. 4, and according to the feature of reaction, reaction distillation column overhead can extraction light component, also can infinite reflux, there is the complicated and high problem of energy consumption of flow process.
Separate tower development and come from Petlyuk tower, the effect integrating by place a vertical next door generation pre-separation tower and king-tower at king-tower interlude, in theory, is embedded in several separable five kinds of even more kinds of components in next door at a tower.For thermal coupling distillation process, pre-separation tower and king-tower link together by gas-liquid flow, and centre is not provided with condenser and reboiler, at the bottom of tower top, tower and sideline product from king-tower extraction, if there is no azeotropic mixture, side line also can obtain high purity product.Compare with serial tower, thermal coupling tower is reduced investment not only, and efficiency is high, because separation component back-mixing in the minimizing of reboiler and condenser and distillation process disappears.CN1177513A has introduced a kind of bulkhead type destilling tower for multicomponent mixture continuous rectification (separating tower), this destilling tower utilization distillation is separated into three kinds or multicomponent more by a mixture, and wherein at least one partition wall is to be detachably arranged in bulkhead type destilling tower.
Therefore, separate tower technology and be applied in reaction distillation process, can substitute reactive distillation column and the solvent recovery tower of traditional handicraft, there is flow process simply and the low feature of energy consumption.
Summary of the invention
Technical problem to be solved by this invention is to need reactive distillation column and product separation tower two towers to realize in current reaction distillation technique, there is flow process complexity and the high problem of energy consumption, provide a kind of new reaction distillation to separate tower tower body, the method has flow process simply and the low feature of energy consumption.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows, a kind of reaction distillation is separated tower tower body, comprise material inlet, tower top charging aperture, tower top discharging opening, charging aperture at the bottom of tower, discharging opening at the bottom of tower, side line is adopted discharging opening, demarcation strip, public rectifying section, conversion zone, extraction side rectifying section, and public stripping section, wherein feed side can arrange rectifying section and/or stripping section, wherein in reaction distillation separation tower tower body, demarcation strip is separated into public rectifying section by tower, feed side rectifying section, conversion zone, feed side stripping section, extraction side rectifying section, and public stripping section, interval at reaction distillation, conversion zone is between feed side rectifying section and feed side stripping section, and conversion zone top is feed side rectifying section, and conversion zone below is feed side stripping section, between demarcation strip top and tower top feed inlet and outlet, region is public rectifying section, and at the bottom of demarcation strip bottom and tower, between feed inlet and outlet, region is public stripping section, and demarcation strip region material inlet opposite side is extraction side rectifying section.
In technique scheme, material inlet is at least one; Material inlet is positioned at reaction distillation interval, and side line is adopted discharging opening and is positioned at extraction side rectifying section; When reaction distillation separation tower is applied to preparing epichlorohydrin through chloropropene epoxidation, public theoretical number of plates of rectifying section is 5～10, public stripping section number of theoretical plate is 8～15, it is 10～30 that conversion zone is equivalent to number of theoretical plate, extraction side theoretical number of plates of rectifying section is 15～30, and the control temperature of conversion zone is 30～60 ℃.
In some reaction distillation process, reactant and product can form three strands of cuts according to boiling point difference, and reactive distillation column can only be cut to two strands of cuts, expect three strands of cuts, must introduce product separation tower.And in some system, reactive distillation column is a realization response function in essence, tower top infinite reflux, reactant and product separation are realized in product separation tower.So traditional handicraft is necessary for the combined process flow of reactive distillation column and product separation tower.In the present invention, reactive distillation column can complete separately reaction distillation and product separation process, realizes the effect of two tower unifications, compares with traditional handicraft, and flow process is simple, and reaction distillation is separated tower alternative reaction destilling tower and product separation tower.Use the present invention in the situation that the operating conditions such as 38～43 ℃ of mass ratio 10: 1, the reaction temperatures of chloropropene and mol ratio 5: 1, solvent and the hydrogen peroxide of hydrogen peroxide, number of theoretical plate 65 are identical, total energy consumption saves 27.7%, has obtained good technique effect.
Accompanying drawing explanation
Fig. 1 is that reaction distillation is separated tower tower body schematic diagram.
Fig. 2 is the A-A view in Fig. 1.
Fig. 3 is the B-B view in Fig. 1.
Fig. 4 is that classical inverse is answered distil process flow chart.
In Fig. 1,2 and 3,1 separates tower for reaction distillation, and 2 is material inlet, 3 tower top discharging openings, 4 is tower top charging aperture, 5 is discharging opening at the bottom of tower, 6 is charging aperture at the bottom of tower, and 7 adopt discharging opening for side line, and 8 is public rectifying section, 9 is feed side rectifying section, 10 is conversion zone, and 11 is feed side stripping section, and 12 is public stripping section, 13 is extraction side rectifying section, and 14 is demarcation strip.
In Fig. 4,1 is reactive distillation column, and 2 is product separation tower, and 3 and 4 is reactant feed, and 5 is light component, and 6 is mixture cut, and 7 is midbarrel, and 8 is heavy distillat.
As shown in Figure 4,3 and 4 reaction raw materials enter reaction distillation charging aperture from the charging aperture of reactive distillation column, in conversion zone reaction, carry out separation, overhead condenser connects tower top feed inlet and outlet, after tower top outlet steam-condensation, carry out infinite reflux, or first sends into tower top import, second portion extraction is as light component 5, and tower reactor mixed fraction 6 enters product separation tower, overhead extraction midbarrel 7, tower reactor obtains heavy distillat 8.
Below by specific embodiment, the present invention is further illustrated, and still, scope of the present invention has more than and is limited to the scope that embodiment covers.
The specific embodiment
[embodiment 1]
Press epichlorohydrin production process shown in Fig. 1, public theoretical number of plates of rectifying section is 10, and public stripping section number of theoretical plate is 15, and it is 25 that conversion zone separative efficiency is equivalent to number of theoretical plate, and extraction side theoretical number of plates of rectifying section is 25.The catalyst of conversion zone filling is SiO
2/ TiO
2the HTS of mol ratio 80, the 1st theoretical plate that 30 % by weight hydrogen peroxide and carbinol mixture (methanol content 70 % by weight) enter conversion zone with 1.00 gram/minute flows (counted from top to bottom, as follows), chloropropene enters from conversion zone bottom respectively with 2.00 gram/minute flows, tower top infinite reflux, side line is from the 10th theoretical plate extraction 2.49 gram/minute of compartmented, all the other are from extraction at the bottom of tower, it is 38～43 ℃ that catalyst reaction section is controlled temperature, after stable operation, in side line extraction stream thigh, there is no epoxychloropropane, at the bottom of tower, extraction is not containing chloropropene and methyl alcohol, overhead condenser energy consumption-0.65 kilojoule/hour, tower bottom reboiler energy consumption be 0.85 kilojoule/hour, the total energy consumption of comparing with comparative example 1 declines 27.7%.
[embodiment 2]
Press reaction distillation shown in Fig. 1 and separate tower tower body, public theoretical number of plates of rectifying section is 5, public stripping section number of theoretical plate is 10, it is 15 that catalyst reaction section separative efficiency is equivalent to number of theoretical plate, extraction side theoretical number of plates of rectifying section is 15, feed side theoretical number of plates of rectifying section is 4, and feed side theoretical number of plates of rectifying section is 6.Catalyst is SiO
2/ TiO
2the HTS of mol ratio 80, the 1st theoretical plate that 30 % by weight hydrogen peroxide and carbinol mixture (methanol content 70 % by weight) enter conversion zone with 1.00 gram/minute flows (counted from top to bottom, as follows), chloropropene enters from catalyst reaction section bottom with 2.00 gram/minute flows, tower top infinite reflux, side line is from the 10th theoretical plate extraction 2.49 gram/minute of compartmented, all the other are from extraction at the bottom of tower, after stable operation, in side line extraction stream thigh, there is no epoxychloropropane, at the bottom of tower, extraction is not containing chloropropene and methyl alcohol, overhead condenser energy consumption-0.69 kilojoule/hour, tower bottom reboiler energy consumption be 0.92 kilojoule/hour.
[embodiment 3]
Press epichlorohydrin production process shown in Fig. 1, public theoretical number of plates of rectifying section is 3, and public stripping section number of theoretical plate is 5, and it is 5 that conversion zone separative efficiency is equivalent to number of theoretical plate, and extraction side theoretical number of plates of rectifying section is 5.The catalyst of conversion zone filling is SiO
2/ TiO
2the HTS of mol ratio 60, 2 % by weight hydrogen peroxide and ethyl acetate mixture (ethyl acetate content 50 % by weight) enter the 1st theoretical plate of conversion zone with 1.00 gram/minute flows, chloropropene enters from catalyst reaction section bottom with 5.00 gram/minute flows, tower top infinite reflux, side line is from the 3rd theoretical plate extraction 5.48 gram/minute of compartmented, all the other are from extraction at the bottom of tower, the weight ratio of first and second portion material is preferably 15: 1, catalyst reaction section temperature is 37～42 ℃, after stable operation, in side line extraction stream thigh, there is no epoxychloropropane, at the bottom of tower, extraction is not containing chloropropene and methyl alcohol, overhead condenser energy consumption-0.73 kilojoule/hour, tower bottom reboiler energy consumption be 0.94 kilojoule/hour.
[comparative example 1]
Press technological process shown in Fig. 4, reactive distillation column theoretical number of plates of rectifying section is 10, and it is 25 that catalyst reaction section separative efficiency is equivalent to number of theoretical plate, and stripping section number of theoretical plate is 10, and product separation tower theoretical number of plates of rectifying section is 30, and stripping section number of theoretical plate is 10.Catalyst is SiO
2/ TiO
2the HTS of mol ratio 80, the 10th theoretical plate that 30 % by weight hydrogen peroxide and carbinol mixture (methanol content 70 % by weight) enter reactive distillation column with 1.00 gram/minute flows (counted from top to bottom, as follows), chloropropene enters from catalyst reaction section bottom with 2.00 gram/minute flows, the infinite reflux of reaction distillation column overhead, reactant and product all enter product separation tower, reflux ratio is 2, after stable operation, in product separation column overhead extraction stream thigh, there is no epoxychloropropane, at the bottom of tower, extraction is not containing chloropropene and methyl alcohol, reactive distillation column overhead condenser energy consumption be-0.38 kilojoule/hour, tower bottom reboiler energy consumption be 0.31 kilojoule/hour, product separation column overhead condenser energy consumption be-0.54 kilojoule/hour, tower bottom reboiler energy consumption be 0.87 kilojoule/hour.
Claims (3)
1. reaction distillation is separated a tower tower body, comprises material inlet, tower top charging aperture, tower top discharging opening, charging aperture at the bottom of tower, discharging opening at the bottom of tower, side line is adopted discharging opening, demarcation strip, public rectifying section, conversion zone, extraction side rectifying section, and public stripping section, wherein feed side arranges rectifying section and/or stripping section, wherein in reaction distillation separation tower tower body, demarcation strip is separated into public rectifying section by tower, feed side rectifying section, conversion zone, feed side stripping section, extraction side rectifying section, and public stripping section; Interval at reaction distillation, conversion zone is between feed side rectifying section and feed side stripping section, and conversion zone top is feed side rectifying section, and conversion zone below is feed side stripping section; Between demarcation strip top and tower top feed inlet and outlet, region is public rectifying section, and at the bottom of demarcation strip bottom and tower, between feed inlet and outlet, region is public stripping section, and demarcation strip region material inlet opposite side is extraction side rectifying section;
Reaction distillation is separated tower and is applied to preparing epichlorohydrin through chloropropene epoxidation, public theoretical number of plates of rectifying section is 5～10, public stripping section number of theoretical plate is 8～15, it is 10～30 that conversion zone is equivalent to number of theoretical plate, extraction side theoretical number of plates of rectifying section is 15～30, and the control temperature of conversion zone is 30～60 ℃.
2. reaction distillation is separated tower tower body according to claim 1, it is characterized in that material inlet is at least one.
3. reaction distillation is separated tower tower body according to claim 1, it is characterized in that material inlet is positioned at reaction distillation interval, and side line is adopted discharging opening and is positioned at extraction side rectifying section.
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| CN102728089B (en) * | 2012-06-18 | 2016-08-10 | 大连理工大学 | Propylene propane fractionation system equipped with lithium bromide absorption type heat pump |
| CN105107220B (en) * | 2015-07-24 | 2016-11-30 | 包头轻工职业技术学院 | Distillation equipment |
| CN106631668B (en) * | 2015-10-28 | 2019-11-15 | 中国石油化工股份有限公司 | Ethylbenzene separation method and ethylbenzene manufacturing processes and the device for producing ethylbenzene and the method using device production ethylbenzene |
| CN105348115B (en) * | 2015-12-23 | 2017-10-20 | 山西翔宇化工有限公司 | A kind of reaction again of rubber antioxidant substandard products and purification processes device |
| US10287222B1 (en) * | 2017-10-20 | 2019-05-14 | Uop Llc | Process and apparatus for desorbent recovery |
| US10377690B1 (en) * | 2018-08-22 | 2019-08-13 | Eastman Chemical Company | Method for catalytic production of refined enal products from an aldehyde feed stream using a single enclosed unit |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1177513A (en) * | 1996-04-30 | 1998-04-01 | 巴斯福股份公司 | Separated-wall type distillation tower for continuous distillation of multi-component mixture |
| CN101244982A (en) * | 2008-01-31 | 2008-08-20 | 中国石油大学(华东) | Hydrolyzation separation apparatus for methyl acetate and technique |
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| TW200738602A (en) * | 2006-02-01 | 2007-10-16 | Asahi Kasei Chemicals Corp | Industrial process for producing high-purity diol |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1177513A (en) * | 1996-04-30 | 1998-04-01 | 巴斯福股份公司 | Separated-wall type distillation tower for continuous distillation of multi-component mixture |
| CN101244982A (en) * | 2008-01-31 | 2008-08-20 | 中国石油大学(华东) | Hydrolyzation separation apparatus for methyl acetate and technique |
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