CN1172735C - Flow-control-free intermittent fine distillation method and apparatus - Google Patents
Flow-control-free intermittent fine distillation method and apparatus Download PDFInfo
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- CN1172735C CN1172735C CNB021350108A CN02135010A CN1172735C CN 1172735 C CN1172735 C CN 1172735C CN B021350108 A CNB021350108 A CN B021350108A CN 02135010 A CN02135010 A CN 02135010A CN 1172735 C CN1172735 C CN 1172735C
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Abstract
The present invention relates to a rectifying method in the operation of basic units in chemical industry, particularly to an intermittent rectifying method and a device thereof without flow control. The device of the present invention provides back flow by a rectifying segment with external partial condensation at the upper part of a rectifying tower. The temperature of the top of the tower is controlled by controlling states of external cooling media. The present invention eliminates the flow control in the operational process formed by object outflow with constant distillation. Moreover, the present invention eliminates liquid holding quantity required for the flow control at the top of the rectifying tower. The transition fraction of the device of the present invention is reduced greatly. Compared with the prior art, the present invention has the advantages of high product purity obtained from rectification, stable quality, and convenient operation and control. The transition fraction can be reduced by more than 20%. Because the present invention has no cool liquid back flow, the heat loss is reduced, the energy consumption for rectifying can be reduced by more than 20%. The present invention is particularly suitable for the separation, the pressure reduction and the intermittent rectification of heat sensitive materials, and intermittent rectification for small tests.
Description
Technical field
The present invention relates to rectificating method and equipment in a kind of chemical engineering unit operation, particularly adopt the batch fractionating method and the equipment of no flow-control.
Background technology
Batch fractionating is a kind of lock out operation that a batch materials is divided into a plurality of fractions by multistage part vaporization and partial condensation, because it can adapt to different materials and separation requirement in same set of equipment, have advantages such as flexibility is strong, reduced investment, in small-scale fine chemistry industry and pharmaceutical industry, be extensive use of.Batch fractionating has two kinds of methods of operating at present, and a kind of is the method for operating that permanent distillate is formed, and it refluxes by continuous increase and recently keeps the composition of distillate, is the main method of operating of the acquisition product of batch fractionating; The 2nd, the method for operating of constant reflux ratio, it is by constant reflux ratio, carries out the transition to the operation of another fraction from a fraction, as the excessive fraction of additional recovery of method one.Form in the operating process at permanent distillate, because reflux ratio is a continually varying, the operation control of load or capacity of returns is had relatively high expectations, it is bigger particularly will to obtain high-quality product difficulty; In the constant reflux ratio operating process, because the liquid holdup of rectifying column top reflux operation equipment is bigger, cause the transition fraction too much, increased the difficulty of separating.Improving these not enough methods is to add tower still volume, increase every batch processing amount, reflux ratio is changed slow down and be easy to control and alleviate cat head and hold the influence that liquid increases the transition fraction, but increase the batch processing amount and not only increase investment, and the increase heat loss, all be extremely disadvantageous particularly to requiring the heat sensitive material rectifying that the lower rectification under vacuum in tower bottoms position or every batch processing time can not be oversize.
Summary of the invention
The purpose of this invention is to provide a kind of efficient batch fractionating method and equipment that reaches easy operating, it adopts the exterior section condensation that backflow is provided at rectifier, not only saved capacity of returns or the load control in the operating process, and eliminated the rectifying column top in order to control the required liquid holdup of flow, the transition fraction is greatly reduced.
The present invention realizes like this, rectifier is changed into rectifying section with exterior section condensation, state by control external refrigeration medium, control the temperature of cat head, thereby the distillate of control cat head is formed or the transition of fraction, the state that is characterized in the cooling medium by control section condensation rectifying section outside has replaced the control of flow, thereby has cancelled flow-control and corresponding apparatus thereof.
Above-described exterior section condensation is that the steam that will rise from the rectifying column still is after rectifying section carries out rectifying, enter exterior section condensation rectifying section, the thermal medium of sending here through thermostat cools off, its interior section condensation number is more than the part evaporating capacity, temperature also progressively reduces, and it reaches required temperature and composition when arriving cat head.The batch distillation process that permanent distillate is formed is operated, because required capacity of returns is ever-increasing, the required thermic load of exterior section condensation rectifying section also is ever-increasing like this, but increase along with separation degree, the distillate that enters the partial condensation rectifying section with higher separating power is formed but constantly decline, temperature constantly rises, and the heat transfer temperature difference of partial condensation rectifying section is constantly increased, and finally causes heat output and capacity of returns to increase automatically.This capacity of returns adaptive ability makes the state control tower top temperature by the control cooling medium become and is more prone to than present flow-control, and the batch fractionating of some system is not even needed control.Batch distillation process operation to perseverance refluxes descends because cat head is formed, and its temperature is constantly to rise, at this time need to improve the temperature of heat of cooling medium, in fact because thermostat is the heat release state, if by adiabatic operation, the heat medium temperature in the thermostat will rise automatically.
The operation of process is become the temperature of control thermostat by the control flow.Because hot cooling medium takes heat to thermostat from exterior section condensation rectifying section, the thermostat heat is increased, keep the temperature of thermostat, just must remove heat with cooling water.Usually can control the temperature of thermostat by the control cooling water, as long as the volume of thermostat is enough, the variations in temperature of thermostat is unhappy, and temperature controlling is not difficult.The transfer of this control is simplified rectifying itself, helps the raising of rectification efficiency and the saving of energy.
The equipment that adopts according to said method comprises rectifying still, rectifying section, exterior section condensation rectifying section, condensate cooler, thermostat and thermal medium circulating pump.Compare with present batch fractionating, it has replaced original overhead condensation recirculation control device with exterior section condensation rectifying section, thermostat and thermal medium circulating pump, and promptly the hot water that comes with thermostat is controlled tower top temperature.
More than said exterior section condensation rectifying section adopt shell and tube, fill efficient separating filler in the tubulation so that the partial condensation rectifying section has very high separating power, the temperature difference at tubulation two ends increases, tower top temperature control is easier.Because the tubulation of partial condensation rectifying section is easy to provide a large amount of separation progression, makes isolated product purity improve greatly, forms high-accuracy separator at intermittence.The height of tubulation is determined according to the height equivalent to one theoretical plate (HETP) of needed number of theoretical plate and filler, 20%～60% of the common desirable full tower number of theoretical plate of number of theoretical plate.Tubulation several reportedly enthusiasm condition and rising gas flow velocity size are determined.
The present invention compares with existing technology, and its outstanding substantive distinguishing features and obvious improvement is:
1, high-accuracy rectifying, separate that the product purity that obtains is higher, quality is more stable.
2, operate and control more convenient, existing batch fractionating is had relatively high expectations to flow-control, and the present invention then only requires the heat of cooling ambient condition that span of control is very little.
3, the transition fraction can reduce more than 20%, adds that no cold liquid refluxes and heat loss reduces, and can reduce the rectifying energy consumption more than 20%.
4, owing to easy to control and transition fraction reduce, can reduce the treating capacity of every batch materials, so not only can reduce tower still volume, and can reduce the processing time of every batch materials, this separation and rectification under vacuum to thermal sensitivity is even more important.
5, to the little batch fractionating device of laboratory, owing to controlling the flow more aspect that becomes.
Description of drawings
Fig. 1 is technological process of the present invention and equipment drawing.
In the technological process shown in Figure 1, the batch fractionating device is made up of rectifying still 1, rectifying section 2, partial condensation rectifying section 3, condensate cooler 4, thermostat 5 and thermal medium circulating pump 6.The top of rectifying still 1 links to each other with rectifying section 2, and the top of rectifying section is partial condensation rectifying section 3, the steam that cat head comes out behind condensate cooler 4 as product.Partial condensation rectifying section 3 is a tubular structure, fills efficient separating filler in managing, and with the thermal medium cooling, hot cooling medium is circulating between the pipe of partial condensation rectifying section 3 and between the thermostat 5 by circulating pump 6 between pipe.
Capital equipment of the present invention is the batch fractionating tower with exterior section condensation, and body of the tower is the cylindrical container of a segmentation, and hypomere is a common rectifying tower section 2; Epimere is an exterior section condensation rectifying section 3, and its structure is a shell and tube, fills efficient separating filler in the tubulation pipe, cools off with thermal medium between pipe.Because the cooling effect of thermal medium, the rising vapor portion in the pipe is condensed, and makes it temperature and progressively descends, steam flow gradually reduces, the content of product slowly rises, as long as control the temperature of suitable heat of cooling medium, just can control required temperature of cat head or composition.
The decision of process conditions: 1, the temperature of hot cooling medium and cat head heat transfer temperature difference are 2～15 ℃, and the temperature difference is more little, and control operation is easy more, but required heat transfer area is big more; 2, the theoretical plate of exterior section condensation rectifying section is 20%～60% of a full tower number of theoretical plate, and full tower number of theoretical plate is Duoed 2～5 than traditional batch fractionating usually; 3, the tubulation height of exterior section condensation rectifying section 3 determines that by the height equivalent to one theoretical plate (HETP) of number of theoretical plate and filler the diameter of tubulation is φ 15mm～φ 40mm.
The specific embodiment
Embodiment one
The recovery of 30% Diluted Alcohol, rectifying section diameter are 0.3 meter, highly are 2.0 meters; The partial condensation section highly is 1.0 meters, tubulation diameter 25mm, the temperature range of thermostat hot water is 72～74 ℃, the control tower top temperature is 78 ℃, the volumetric concentration of recovered alcohol keeps 95%, the rate of recovery of alcohol reaches 98%, and the volumetric concentration of common batch fractionating recovered alcohol is 93%, and the rate of recovery of alcohol is about 94%.
Embodiment two
Adopt batch fractionating to reclaim methyl alcohol from 50% methanol aqueous solution, the rectifying section diameter is 0.2 meter, highly is 1.0 meters; The partial condensation section highly is 0.6 meter, tubulation diameter 20mm, the temperature of thermostat hot water is 60～62 ℃ of scopes, the control tower top temperature is 64.5 ℃, the concentration of product methyl alcohol keeps 99%, yield is about 96%, and the concentration of common batch fractionating methanol product is maintained 97%, and yield is about 93%.
Embodiment three
The batch fractionating experimental provision that ethanol-ethyl lactate system is separated, the partial condensation rectifying section is one 24 mouthfuls, the condenser west tube of 400mm, the high 250mm of rectifying section, the temperature range of thermostat hot water is 74～76 ℃, the control tower top temperature is 78 ℃, the overhead product concentration of ethanol is 98%, and the concentration of tower still product ethyl lactate is 99%, and the concentration of common batch fractionating ethyl lactate product is about 97%.
Claims (4)
1, a kind of batch fractionating method it is characterized in that the rectifier employing has the exterior section condensation backflow is provided, thereby saved volume control device, and the temperature at rectifying column top and composition is just controlled by the temperature of the cooling medium of thermostat conveying.
2, method according to claim 1 is characterized in that the exterior section condensation is the rising steam with entering part condensation rectifying section, and the thermal medium of sending here by thermostat carries out external refrigeration, produces partial condensation, and condensate liquid is as the backflow of rectifying.
3, the equipment that adopted of the described batch fractionating method of a kind of claim 1 is characterized in that equipment is made up of rectifying still (1), rectifying section (2), exterior section condensation rectifying section (3), condensate cooler (4), thermostat (5), thermal medium circulating pump (6).The top of rectifying still (1) links to each other with rectifying section (2), the top of rectifying section (2) is exterior section condensation rectifying section (3), exterior section condensation rectifying section (3) below has outlet to lead to thermostat (5), connect circulating pump (6) from thermostat (5), the outlet of circulating pump (6) leads to the top of exterior section condensation rectifying section (3), exterior section condensation rectifying section (3) top exit pipe connects condensate cooler (4), the steam that cat head comes out behind condensate cooler (4) as product.Exterior section condensation rectifying section (3) is circulating between the pipe of partial condensation rectifying section (3) and between the thermostat (5) by circulating pump (6) with thermal medium cooling, hot cooling medium.
4, according to the equipment that claim 3 adopted, exterior section condensation rectifying section (3) adopts shell and tube, and the diameter of tubulation is φ 15mm～φ 40mm, fills efficient separating filler in the tubulation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021350108A CN1172735C (en) | 2002-10-21 | 2002-10-21 | Flow-control-free intermittent fine distillation method and apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021350108A CN1172735C (en) | 2002-10-21 | 2002-10-21 | Flow-control-free intermittent fine distillation method and apparatus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1404896A CN1404896A (en) | 2003-03-26 |
| CN1172735C true CN1172735C (en) | 2004-10-27 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB021350108A Expired - Fee Related CN1172735C (en) | 2002-10-21 | 2002-10-21 | Flow-control-free intermittent fine distillation method and apparatus |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102039059B (en) * | 2009-10-10 | 2012-11-07 | 中国石油化工股份有限公司 | Method for controlling top of fine propylene tower |
| CN102974115B (en) * | 2012-12-18 | 2014-07-23 | 济南大学 | Automatic control fractionation device and application thereof |
| CN111450561B (en) * | 2020-04-15 | 2024-04-26 | 陕西聚能新创煤化科技有限公司 | Energy-saving carrier gas stripping system and stripping process |
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