CN101053815A - Hot reflux tower for producing carbon-13 - Google Patents
Hot reflux tower for producing carbon-13 Download PDFInfo
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- CN101053815A CN101053815A CN 200610073082 CN200610073082A CN101053815A CN 101053815 A CN101053815 A CN 101053815A CN 200610073082 CN200610073082 CN 200610073082 CN 200610073082 A CN200610073082 A CN 200610073082A CN 101053815 A CN101053815 A CN 101053815A
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Abstract
A hot reflux tower for producing carbon-13 belongs to a chemical reaction device art. The invention discloses a hot reflux tower for producing carbon-13, which mainly comprises the following five parts from above to below: a tower top cover with a calandria liquid distributors, a direct heat exchange-cold liquid leaching tower section filling with structured packing, a decoposing tower section, a cellpacking standing heater tower pot and a tower bottom cap, wherein the heat travels regularly in a shell pass, and the working material runs along a pipe pass. Decomposition products of the hot reflux are carbon dioxide and solution of di-n-butylamine/octane which flows out from the bottom of the tower pot, and the carbon dioxide flows out from the top of the tower top cover. The invention replaces an expensive cellpacking standing gas cooler of the existing technology by the direct heat exchange-cold liquid leaching tower section filling with structured packing, and is provided with a temperature control component for controlling decomposition temperature at 60 +/-5 DEG C., which precision of the control temperature is not +/- 1 DEG C. but +/- 5 DEG C. Accordingly, energy consumption is saved about 20%, in addition to saving the investment cost, and crystallization accident is avoided.
Description
Technical field
The present invention relates to cold and hot backflow carbon dioxide/di-n-butylamine/octane isotope exchange produces the hot reflux tower that uses in high dense carbon-13 technology, belongs to the chemical reaction device field.
Background technology
Produce in high dense carbon-13 method in cold and hot backflow carbon dioxide/di-n-butylamine/octane isotope exchange, the hot reflux reaction is one of key technology.Described hot reflux reaction is that carbamate/octane solution decomposes that isotope exchange column in the Self-cascading production system flows out is become the process of carbon dioxide and di-n-butylamine/octane solution.The hot reflux tower of prior art is to establish a packing tower section above the vertical heating kettle of shell, claim the decomposition tower section, section overhead one thermometer, above described decomposition tower section, be the shell upright radiator, decomposition temperature need be controlled at 70 ± 1 ℃, because ± 1 ℃ accuracy of temperature control is difficult for grasping, under described hot reflux tower version situation, when operating temperature exceeds 1～2 ℃ of the described temperature control upper limit slightly, will on the cooler tubulation inwall of described decomposition tower section white crystals appear, stop up gas channel when serious, cause the parking accident.This is a technical barrier of realizing that described carbon-13 production process needs to be resolved hurrily.
Summary of the invention
In order to solve above-mentioned technical barrier, the hot reflux tower stable operation is reliable in the assurance system, the invention provides a kind of hot reflux tower that carbon-13 is produced that is used for, it is characterized in that, described hot reflux tower mainly is divided into cap five major parts at the bottom of cat head, direct heat exchange-cool liquid eluting column section, decomposition tower section, heating tower's still, the tower from top to bottom, between described five major parts by flange fixedly connected, its by
Be filled with structured packing in the tower body of described direct heat exchange-cool liquid eluting column section, form direct heat exchange-cool liquid drip washing section packing layer;
Below described direct heat exchange-cool liquid drip washing section packing layer, the position of described decomposition tower section top, be provided with measure and the control decomposition temperature 60 ± 5 ℃ temperature control element;
In the tower body side of described decomposition tower section, be provided with the recirculating still liquid entrance sleeve that is used for the cycling of still liquid near described decomposition tower section and heating tower's still joint;
The cap bottom is provided with and is used for the recirculating still liquid discharge connection that the cycling of still liquid is used at the bottom of described tower.
As in further improvement of the present invention, the height of described direct heat exchange-cool liquid drip washing section packing layer is 300～600mm, and operating pressure is gauge pressure 0.01～0.03Mpa, and liquid spraying density is 0.5～5ml/cm
2.min.
As in further improvement of the present invention, described top of tower branch comprises tower top cover, the carbon dioxide vent that is located at described tower top cover top center place is taken over, the liquid-inlet that is located at described tower top cover side is taken over, and is located in the described tower top cover and the calandria liquid distribution trough that is connected with described liquid-inlet adapter.
As in further improvement of the present invention, described calandria liquid distribution trough has the person in charge and the comb that is interconnected, described comb is arranged symmetrically in the horizontal both sides of the described person in charge, described comb below has equally distributed liquid spraying aperture, aperture 1.5～3mm, liquid spraying density are 150～200 holes/m
2
As in further improvement of the present invention: only the outside of cap three parts is enclosed with heat-insulation layer at the bottom of decomposition tower section, heating tower's still, the tower.
As in further improvement of the present invention, described decomposition tower section bed stuffing height is 500～900mm, and operating pressure is gauge pressure 0.01～0.03Mpa, and liquid spraying density is 0.5～5ml/cm2.min.
As in further improvement of the present invention, described heating tower's still adopts the vertical heating tower's still of shell, and shell side is walked low pressure heating steam, and tube side is a hydraulic fluid; The side, housing top of described heating tower's still is provided with the heating steam entrance sleeve, and side, housing below is provided with the condensate water discharge connection.
Adopt hot reflux tower of the present invention, can successfully realize cold and hot backflow carbon dioxide/di-n-butylamine/high dense carbon-13 process of octane isotope exchange production, and part producing cost, the energy consumption of also having saved part investment cost and about 20% have simultaneously been reduced.
Description of drawings
Fig. 1. be the structural representation of an exemplary embodiments of the present invention.
The specific embodiment
Describe the present invention in detail below in conjunction with drawings and Examples.
As shown in Figure 1, in exemplary embodiments of the present invention, the described hot reflux tower that is used to produce carbon-13 mainly is divided into cap five major parts at the bottom of cat head, direct heat exchange-cool liquid eluting column section, decomposition tower section, heating tower's still, the tower from top to bottom, and is fixedly connected by flange between described five major parts.In the present embodiment, only the outside of cap three parts is enclosed with heat-insulation layer 25 at the bottom of decomposition tower section, heating tower's still, the tower, and heat-insulation layer is not established in direct heat exchange-cool liquid eluting column section outside, so that utilize the air cooling.
Described top of tower branch comprises tower top cover 19, the carbon dioxide vent that is located at tower top cover 19 top center places takes over 20, the liquid-inlet that is located at tower top cover 19 sides is taken over 21 (entering for carbamate/octane solution to be decomposed), be located at the tower top cover flange 18 of tower top cover 19 bottoms, and be located in the tower top cover 19 and and take over the 21 calandria liquid distribution troughs that are connected with liquid-inlet.Described calandria liquid distribution trough has the person in charge 22 and the comb 23 that is interconnected, and comb 23 is arranged symmetrically in is responsible for 22 horizontal both sides, and comb 23 belows have equally distributed liquid spraying aperture, and aperture 1.5～3mm, liquid spraying density are 150～200 holes/m
2On the direct heat exchange-cool liquid drip washing packing layer that the carbamate/octane solution that enters described hot reflux tower top is assigned to equably hereinafter will describe, raising enters the cold carbamate/octane solution of hot reflux tower and carries out the gas/liquid effect of direct contact heat exchange mutually with the hot carbon dioxide that leaves described decomposition tower section (carbon dioxide of heat is the catabolite after carbamate/octane solution is heated), also can improve simultaneously the effect that cold carbamate/octane solution is washed the little crystallization of micro-carbamate of carrying secretly in the described hot carbon dioxide, these micro-crystallizations are malfunctioning and produce because of temperature control once in a while.Flow rate of liquid can be controlled in 0.2～0.3m/s in described calandria liquid distribution trough was responsible for, and flow rate of liquid can be controlled in 0.15～0.2m/s in the comb of described calandria liquid distribution trough, to guarantee that liquid distribution is even.
The tower body 15 of described direct heat exchange-cool liquid eluting column section is columnar, fixedlying connected with tower top cover flange 18 by direct heat exchange-cool liquid drip washing section upper flange 17 in its upper end, fixedlys connected with a decomposition section upper flange 13 (hereinafter describing) by direct heat exchange-cool liquid drip washing section lower flange 14 in its lower end.Be filled with structured packing in the tower body 15 of direct heat exchange-cool liquid eluting column section, form direct heat exchange-cool liquid drip washing section packing layer 16, bed stuffing height is 300～600mm, and operating pressure is gauge pressure 0.01～0.03Mpa, and liquid spraying density is 0.5～5ml/cm
2.min.The present invention gets and has replaced the vertical carbon dioxide cooler of the shell that cost is more expensive in the prior art with the not high packing section (being direct heat exchange-cool liquid drip washing section packing layer) that only is 300～600mm, the expense of not only reducing investment outlay, and can also energy efficient, the more important thing is owing to utilize and newly to be added to of the drip washing of hot reflux tower cold soln to be decomposed the hot carbon dioxide that comes out from the decomposition tower section, can dissolve the micro-crystallization of carrying secretly once in a while in the described hot carbon dioxide, therefore the accident of having stopped the crystallization blocking channel takes place, and has guaranteed that production process carries out smoothly.Because gas-liquid two-phase is directly to contact in the enough flourishing packing layer of specific surface, heat exchange best results (be all dividing wall type heat exchangers can't be obtained), therefore the carbon dioxide temperature of leaving described direct heat exchange-cool liquid drip washing section packing layer has dropped to room temperature, the next step that directly can be used for production process, owing to do not had to use water-cooled shell and tube cooler, the energy consumption that just can save down this part cooling water naturally; Because solution to be decomposed has reclaimed the heat of hot carbon dioxide and by the intensification preheating, has alleviated the burden of heating tower's still, can reduce part heating steam consumption; Experimental results show that 60 ± 5 ℃ of decomposition temperatures are identical with 70 ± 1 ℃ decomposition effect, the decomposition tower still flows out that residual carbon dioxide content all can reach in the liquid≤requirement of 5ppm, owing to lowered nearly 10 ℃ decomposition temperature, can reduce part heating steam consumption again, through the about energy efficient 20% of measuring and calculating the present invention.
Below the packing layer in the tower body 15 of direct heat exchange-cool liquid eluting column section, the position of decomposition tower section top, be provided with measure and the control decomposition temperature 60 ± 5 ℃ temperature control element 24, temperature control element 24 stretches into center, packing layer below in the direct heat exchange-cool liquid eluting column section tower body 15 from direct heat exchange-cool liquid eluting column section tower body 15 sides, be used at 60 ± 5 ℃ of heating steam flows that the scope inner control is required.Since temperature control precision from prior art ± 1 ℃ change into ± 5 ℃, required control instrument investment cost also has tangible reduction.
The tower body 11 of described decomposition tower section is a cylindrical shape, and its upper end is connected with direct heat exchange-cool liquid drip washing section lower flange 14 by decomposing section upper flange 13, and its lower end is by decomposing section lower flange 9 and upper perforated plate 8 (hereinafter describing).Be filled with structured packing in the tower body 11 of decomposition tower section, form and decompose section packing layer 12, bed stuffing height is 500～900mm, and operating pressure is gauge pressure 0.01～0.03Mpa, and liquid spraying density is 0.5～5ml/cm
2.min.In tower body 11 sides of decomposition tower section, be provided with the recirculating still liquid entrance sleeve 10 that is used for the cycling of still liquid near decomposition tower section and heating tower's still joint.
Described heating tower's still adopts the vertical heating tower's still of shell, and shell side is walked low pressure heating steam, and tube side is a hydraulic fluid.Described heating tower's still comprises cylindrical shape heating tower still shell body 5, is separately fixed at the upper perforated plate 8 and the lower perforated plate 4 of cylindrical shape heating tower still shell body 5 top and bottom, and is located at the heating tubulation 6 in the middle of the described upper and lower tube sheet.Side, heating tower's still shell body 5 top is provided with heating steam entrance sleeve 7 near upper perforated plate 8 places, side, heating tower's still shell body 5 below is provided with condensate water discharge connection 26 near lower perforated plate 4 places, and condensate water discharge connection 26 is positioned at the offside of heating steam entrance sleeve 7.Heating steam from the housing upper side to entering, condensate water by the housing lower side to discharge.
Owing to be provided with recirculating still liquid entrance sleeve 10 and the recirculating still liquid discharge connection 27 used for still liquid cycling in the production process in the present invention, therefore reduced the solvent make-up amount of expensive periodic duty solution significantly, and make production process more stable, improved the concentrated effect of carbon-13.
The above only is an exemplary embodiments of the present invention, not in order to restriction the present invention, all any modifications of being done within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. one kind is used for the hot reflux tower that carbon-13 is produced, it is characterized in that, described hot reflux tower mainly is divided into cap five major parts at the bottom of cat head, direct heat exchange-cool liquid eluting column section, decomposition tower section, heating tower's still, the tower from top to bottom, and is fixedly connected by flange between described five major parts, wherein
Be filled with structured packing in the tower body of described direct heat exchange-cool liquid eluting column section, form direct heat exchange-cool liquid drip washing section packing layer;
Below described direct heat exchange-cool liquid drip washing section packing layer, the position of described decomposition tower section top, be provided with measure and the control decomposition temperature 60 ± 5 ℃ temperature control element;
In the tower body side of described decomposition tower section, be provided with the recirculating still liquid entrance sleeve that is used for the cycling of still liquid near described decomposition tower section and heating tower's still joint;
The cap bottom is provided with and is used for the recirculating still liquid discharge connection that the cycling of still liquid is used at the bottom of described tower.
2. hot reflux tower according to claim 1 is characterized in that: the height of described direct heat exchange-cool liquid drip washing section packing layer is 300～600mm, and operating pressure is gauge pressure 0.01～0.03Mpa, and liquid spraying density is 0.5～5ml/cm
2.min.
3. hot reflux tower according to claim 1, it is characterized in that: described top of tower branch comprises tower top cover, the carbon dioxide vent that is located at described tower top cover top center place is taken over, the liquid-inlet that is located at described tower top cover side is taken over, and is located in the described tower top cover and the calandria liquid distribution trough that is connected with described liquid-inlet adapter.
4. hot reflux tower according to claim 3, it is characterized in that: described calandria liquid distribution trough has the person in charge and the comb that is interconnected, described comb is arranged symmetrically in the horizontal both sides of the described person in charge, described comb below has equally distributed liquid spraying aperture, aperture 1.5～3mm, liquid spraying density are 150～200 holes/m
2
5. hot reflux tower according to claim 1 is characterized in that: only the outside of cap three parts is enclosed with heat-insulation layer at the bottom of decomposition tower section, heating tower's still, the tower.
6. hot reflux tower according to claim 1 is characterized in that: described decomposition tower section bed stuffing height is 500～900mm, and operating pressure is gauge pressure 0.01～0.03Mpa, and liquid spraying density is 0.5～5ml/cm2.min.
7. hot reflux tower according to claim 1 is characterized in that: described heating tower's still adopts the vertical heating tower's still of shell, and shell side is walked low pressure heating steam, and tube side is a hydraulic fluid; The side, housing top of described heating tower's still is provided with the heating steam entrance sleeve, and side, housing below is provided with the condensate water discharge connection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006100730828A CN101053815B (en) | 2006-04-13 | 2006-04-13 | Hot reflux tower for producing carbon-13 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006100730828A CN101053815B (en) | 2006-04-13 | 2006-04-13 | Hot reflux tower for producing carbon-13 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101053815A true CN101053815A (en) | 2007-10-17 |
| CN101053815B CN101053815B (en) | 2010-08-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2006100730828A Expired - Fee Related CN101053815B (en) | 2006-04-13 | 2006-04-13 | Hot reflux tower for producing carbon-13 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103611489A (en) * | 2013-11-26 | 2014-03-05 | 四川科新机电股份有限公司 | Multifunctional heat transfer separation unit |
| CN103638882A (en) * | 2013-11-21 | 2014-03-19 | 内蒙古伊泰煤制油有限责任公司 | Quick cooling method and system of internal heat exchange column tube of fischer-tropsch synthesis reactor |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1053881C (en) * | 1996-03-20 | 2000-06-28 | 中国石油化工总公司 | Method for separation of cracking C5 fraction |
| US6070431A (en) * | 1999-02-02 | 2000-06-06 | Praxair Technology, Inc. | Distillation system for producing carbon dioxide |
| CN1162380C (en) * | 2001-10-12 | 2004-08-18 | 中国石油化工股份有限公司 | Separation method of cracked C5 fraction |
| CN1190405C (en) * | 2002-05-15 | 2005-02-23 | 中国科学院工程热物理研究所 | Energy saving separation technology of refining dimethyl ether and recovery carbon dioxide at the same time |
-
2006
- 2006-04-13 CN CN2006100730828A patent/CN101053815B/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103638882A (en) * | 2013-11-21 | 2014-03-19 | 内蒙古伊泰煤制油有限责任公司 | Quick cooling method and system of internal heat exchange column tube of fischer-tropsch synthesis reactor |
| CN103638882B (en) * | 2013-11-21 | 2015-12-23 | 内蒙古伊泰煤制油有限责任公司 | A kind of Fischer-Tropsch synthesis device internal heat tubulation fast cooling method and system |
| CN103611489A (en) * | 2013-11-26 | 2014-03-05 | 四川科新机电股份有限公司 | Multifunctional heat transfer separation unit |
| CN103611489B (en) * | 2013-11-26 | 2016-03-16 | 四川科新机电股份有限公司 | Multifunctional heat transfer separation unit |
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| Publication number | Publication date |
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| CN101053815B (en) | 2010-08-11 |
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Granted publication date: 20100811 Termination date: 20120413 |