CN101279144A - Double boiler intermittent extraction and rectification device for separating alcohol-water azeotropy system and method - Google Patents
Double boiler intermittent extraction and rectification device for separating alcohol-water azeotropy system and method Download PDFInfo
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- CN101279144A CN101279144A CNA2007100601588A CN200710060158A CN101279144A CN 101279144 A CN101279144 A CN 101279144A CN A2007100601588 A CNA2007100601588 A CN A2007100601588A CN 200710060158 A CN200710060158 A CN 200710060158A CN 101279144 A CN101279144 A CN 101279144A
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Abstract
The invention relates to a double reactor interrupted extraction and rectifying device and a method of a separation ethanol-water azeotropy system. The device of the invention essentially comprises a material reactor, a solvent recycling reactor, an intermediate storage tank, a rectifying tower, a condenser, a product collecting tank, and a solvent constant temperature storage tank; the method of the invention comprises the total-reflux operation without solvents, the total-reflux operation with fresh solvents, the recovery of the constant reflux ratio with the fresh solvents, the total-reflux operation without the solvents, the total-reflux operation with the fresh solvents and the recycling solvents, the recovery of the constant reflux ratio with the fresh solvents and the recycling solvents, the constant reflux ratio operation without the solvents, and solvent recycling. The bottom part of a tower of the invention is provided with a solvent recycling system; the solvents are recycled when the interrupted extraction and rectifying process is conducted, and the recycled solvents return to the tower for cycling operation, therefore, the volume and the heat load of a tower reactor are greatly reduced, and the goal of reasonably utilizing the solvents is realized.
Description
Technical field
The present invention relates to batch extracting rectified technology, particularly a kind of double-kettle batch extraction rectification device of separating ethanol-water azeotropic system and method are the method with the solvent pairs import double-kettle batch extraction rectifying separating ethanol-water azeotropic system that adopts batch fractionating system and solvent recovery system to combine specifically.
Background technology
Extracting rectifying (Extractive Distillation, ED) be on the basis of conventional distillation, to add suitable the 3rd component-extractant (also claiming solvent), with the relative volatility between the separated key component (solute) in the change rectifying column, thereby make difficult separation mixture change easily separated system into.Can be divided into according to the mode of operation extracting rectifying: continuous extraction rectifying and batch extracting rectified.At present, the extracting rectifying separating technology is widely used in chemical industry production with the form of continuous rectification substantially, but its shortcoming is to need special solvent recovery tower, and equipment investment is bigger.Since Berg in 1985 since (2) propose in batches the extracting rectifying mode, extraction and distillation technology has had bigger development again, batch extracting rectified technology combines the advantage of batch fractionating and extracting rectifying: equipment investment is little, and it is a plurality of products that the tower that available relative continuous rectification is tried one's best few separates multicomponent mixture.For medication chemistry, the system of the smaller and difficult separation of some the batch processing amounts in the fine chemistry industry is generally selected for use batch extracting rectified.Traditional batch extracting rectifying mode of operation can be divided into: solvent once adds mode and the semicontinuous adding mode of solvent.Lang (7) and Yatim (8) etc. have carried out systematic research to the batch extracting rectified pattern of the semicontinuous adding pattern of solvent, have proposed typical FOUR EASY STEPS step and corresponding optimisation strategy thereof:
(1) total reflux operation under the solvent-free adding;
(2) add total reflux operation under the solvent continuously, purification rectifying section product;
(3) add finite reflux operation under the solvent continuously, the extraction product;
(4) distillation operation under the solvent-free adding separates solvent.
This pattern has now become conventional batch extracting rectified typical module.
Yet in this mode of operation, along with constantly carrying out of batch fractionating, solvent constantly adds, and makes tower still institute hydrops body more and more, and is very big to the volume requirement of tower still.Simultaneously because high boiling solvent constantly joins the tower still, make must produce stable rising steam and become very difficult, need continue to increase the heat that adds of tower still.This mode of operation is had relatively high expectations to the volume and the thermic load of tower still, and can not guarantee stable steam flow rate in the later stage, and reasonable inadequately to the utilization of solvent and heat.
Summary of the invention
The object of the present invention is to provide a kind of double-kettle batch extraction rectification device and method of separating ethanol-water azeotropic system, adopt the double-kettle batch extraction rectification device separating ethanol-water azeotropic system of solvent pairs import, in the bottom of tower in conjunction with a solvent recovery system, in batch extracting rectified, reclaim solvent, and institute's recovered solvent is added back to again carries out cycling in the tower, thereby significantly reduced the volume and the thermic load of tower still, and reached the purpose of the reasonable utilization of solvent.
The double-kettle batch extraction rectification device of separating ethanol-water azeotropic system provided by the invention mainly comprises: raw material still and solvent recovery still, intermediate storage tank, rectifying column, condenser, product collecting tank, solvent constant temperature storage tank; And supporting filler and tower internals, pump, thermocouple and rotor flow note.
Connected mode: the raw material still is connected by intermediate storage tank with the solvent recovery still, be connected with triple valve in the middle of rectifying column, raw material still, the intermediate storage tank, top of tower is connected with condenser, is connected with trap on the condenser, and tower body and solvent recovery still all are connected with the product collecting tank.
Two stills of described raw material still and solvent recovery still were controlled with being connected by valve of rectifying column;
Described rectifying column is a metal stainless steel system, interior dress stainless steel Dixon ring filler.Rectifying column has fresh solvent inlet and recovery solvent to add inlet on one's body respectively, reclaims solvent and adds inlet below fresh solvent adds inlet.
Described fresh solvent adds inlet and is-300mm apart from cat head, reclaims solvent and adds inlet and add inlet apart from fresh solvent and be-550mm, apart from the bottom of the tower being-1150mm.
Described raw material still volume is 30L, and the solvent recovery still is 20L, all adopts heat-conducting oil heating.
The volume of the product jar of described intermediate storage tank and solvent recovery still all is 10L.
The method that the invention provides separating ethanol-water azeotropic system may further comprise the steps:
1) total reflux operation under the solvent-free adding
In the described raw material still of the disposable adding of alcohol-water raw material, close and connect solvent recovery system valve, open and connect batch fractionating system valve, make solvent recovery system and batch fractionating system isolated, in the batch fractionating system, carry out the normal pressure total reflux operation;
2) total reflux operation of fresh solvent under adding arranged
Total reflux operation adds inlet from the fresh solvent near cat head and adds fresh solvent after a period of stabilisation, and this moment, shut off valve 8 was opened valve 9, made the solvent of phegma and adding all enter intermediate storage tank, still carried out total reflux operation.
3) there is fresh solvent to decide the reflux ratio extraction under adding
In step 2) total reflux operation after a period of stabilisation, survey the concentration of cat head extraction product, reach after the extraction requirement with reflux ratio extraction in 1: 1.After the accumulation of fluid in the middle storage tank arrives to a certain degree, put it in the solvent recovery still.The solvent recovery still carries out simple distillation with bigger power heating, steams light component quickly, and the steam that is rich in light component enters the product jar 5 of tower bottom after condenser 7 condensations, and the liquid that remains in the solvent recovery jar is recovered solvent.This moment, the batch fractionating system still was in the stage of deciding the reflux ratio extraction.
4) total reflux operation under the solvent-free adding
When the temperature of solvent recovery still is elevated to uniform temperature, in the tower steam quantitative change seldom after, stop the heating of solvent recovery still.After this at first stop the adding of fresh solvent, with the liquid in the product jar 5, the disposable raw material still of putting into, valve-off is total reflux operation then.
5) fresh solvent and the total reflux operation of reclaiming under the solvent adding are arranged
Recovered solvent in the solvent recovery still is migrated out still, and constant temperature is in a certain temperature, and after infinite reflux was stable, shut off valve 9 was opened valve 8, and flow liquid is entered in the intermediate storage tank, and solvent after the recovery and fresh solvent add in the tower with certain speed respectively.The batch fractionating system is kept total reflux operation.
6) fresh solvent and reclaim solvent and decide the reflux ratio extraction under adding is arranged
After overhead fraction reaches qualified requirement, with certain reflux ratio extraction.
After this step repeats II (4), 5 exactly), 6) step, after cat head extraction product is defective, stops solvent and add, at last with the solvent recovery still, intermediate storage tank and recovered solvent add the raw material still and are recovered to high boiling solvent, and this operating process so far finishes.
The present invention has several important feature:
(1) adopt two stills to replace single tower still at the bottom of the tower.One of them tower still carries out the batch fractionating operation as the raw material still, and another one tower still carries out the solvent recovery operation as the solvent recovery still.Two tower stills link to each other with rectifying column by valve 8,9 respectively.
(2) adopt a plurality of solvents to add the body of the tower design of inlet.Have fresh solvent to add inlet at top of tower, simultaneously fresh solvent add inlet below have the solvent of recovery to add inlet.
(3) fresh solvent and reclaim solvent and add extracting rectifying down simultaneously and operate is arranged.Adding speed by control fresh solvent and recovery solvent reaches optimum efficiency.Saved the addition of fresh solvent simultaneously.
(4) will need the operation of two rectification systems to be incorporated in the individual system originally, save device fabrication cost and running cost.The volumetric loading and the thermic load of raw material still have been reduced simultaneously.
Batch extracting rectified method of operating before the double-kettle batch extraction rectifying new method of employing solvent pairs provided by the invention import is compared has tangible advantage.Solvent does not directly enter the raw material still, has so just guaranteed that the volume of raw material still can be very not big, and the not too large easy operation of the fluctuation of still temperature.Recovered solvent adds the consumption that the tower still has reduced fresh solvent once more from tower simultaneously.After adopting new mode of operation, solvent recovery still and solvent recovery still have been shared the volumetric loading of raw material still, and making does not need to consider especially the influence of solvent adding amount to still when carrying out the design of solvent recovery still, for the design of tower provides very big flexibility.The solvent recovery still has also been shared the thermic load of raw material still simultaneously, has reduced the raw material still and has added the difficulty that heat is regulated and control, and tower still rising quantity of steam is kept relative stability in operating process.
Description of drawings
Fig. 1 is an Experimental equipment of the present invention.
The specific embodiment
Reaching embodiment in conjunction with the accompanying drawings is illustrated of the present invention.
Among Fig. 1: install the metal stainless steel system that designs into voluntarily, equipment mainly is made of two stills, extraction section, rectifying section, condenser, solvent circulation, product jar, intermediate storage tank and blind controller system.
1-raw material still; 2-solvent recovery still; The 3-intermediate storage tank; 4,5-product jar; 6,7-condenser; 8,9-valve.Solvent recovery still 2, intermediate storage tank 3, product jar 5, condenser 7 is formed solvent recovery unit; Raw material still 1, product jar 4, condenser 6, valve 8 and valve 9 are formed the batch fractionating device.
(1) volume of raw material still 1 is 30L, and solvent recovery still 2 is 20L, all adopts heat-conducting oil heating, and thermocouple is equipped with in inside, and the raw material still links to each other with U type pipe differential water pressures meter;
(2) the tower body internal diameter is 89mm, and the stainless steel Dixon ring filler of interior dress Φ 3mm * 3mm because two cover solvent circulation are arranged, so body of the tower is divided into three sections, is a rectifying section more than the fresh solvent inlet, long 300mm; Reclaiming below the colvent inlet is extraction section, and long is 1150mm; And be extraction section with respect to top rectifying section between two sections, and with respect to the following rectifying section that just can be understood as, longly be 550mm.We can classify like this, and body of the tower from top to bottom is respectively: rectifying section, extraction section I and extraction section II.Every section is all adopted rock wool heat-preservation.
(3) distributor is arranged above the body of the tower, outside by pipeline connection reflux ratio magnetic valve, regulate the extraction of overhead.
(4) cat head is installed shell and tube condenser 6, makes to be cooled with circulating water, and condenser top is equipped with trap, prevent since in the tower steam rise too fast and can not total condensation, in order to avoid loss of material.
(5) volume of the product jar 5 of intermediate storage tank 3 and solvent recovery still all is 10L and has liquid level gauge, need not take out liquid like this and just can directly read volume, and is very directly perceived, convenient.
The method that the invention provides separating ethanol-water azeotropic system may further comprise the steps:
1) total reflux operation under the solvent-free adding
In the described raw material still of the disposable adding of alcohol-water raw material, valve-off 9 is opened valve 8, makes solvent recovery system and batch fractionating system isolated, carries out the normal pressure total reflux operation in the batch fractionating system;
2) total reflux operation of fresh solvent under adding arranged
Total reflux operation adds inlet from the fresh solvent near cat head and adds fresh solvent after a period of stabilisation, and this moment, shut off valve 8 was opened valve 9, made the solvent of phegma and adding all enter intermediate storage tank, still carried out total reflux operation.
3) there is fresh solvent to decide the reflux ratio extraction under adding
In step 2) total reflux operation after a period of stabilisation, survey the concentration of cat head extraction product, reach after the extraction requirement with reflux ratio extraction in 1: 1.After the accumulation of fluid in the middle storage tank arrives to a certain degree, put it in the solvent recovery still.The solvent recovery still carries out simple distillation with bigger power heating, steams light component quickly, and the steam that is rich in light component enters the product jar 5 of tower bottom after condenser 7 condensations, and the liquid that remains in the solvent recovery jar is recovered solvent.This moment, the batch fractionating system still was in the stage of deciding the reflux ratio extraction.
4) total reflux operation under the solvent-free adding
When the temperature of solvent recovery still is elevated to uniform temperature, in the tower steam quantitative change seldom after, stop the heating of solvent recovery still.After this at first stop the adding of fresh solvent, with the liquid in the product jar 5, the disposable raw material still of putting into, valve-off is total reflux operation then.
5) fresh solvent and the total reflux operation of reclaiming under the solvent adding are arranged
Recovered solvent in the solvent recovery still is migrated out still, and constant temperature is in a certain temperature, and after infinite reflux was stable, shut off valve 9 was opened valve 8, and flow liquid is entered in the intermediate storage tank, and solvent after the recovery and fresh solvent add in the tower with certain speed respectively.The batch fractionating system is kept total reflux operation.
6) fresh solvent and reclaim solvent and decide the reflux ratio extraction under adding is arranged
After overhead fraction reaches qualified requirement, with certain reflux ratio extraction.
After this step repeats II (4), 5 exactly), 6) step, after cat head extraction product is defective, stops solvent and add, at last with the solvent recovery still, intermediate storage tank and recovered solvent add the raw material still and are recovered to high boiling solvent, and this operating process so far finishes.
Application Example
Selecting for use the water-ethanol binary azeotrope to be the experiment system, is the extraction solvent with ethylene glycol.Experimental provision is the metal tower of internal diameter 89mm, and body of the tower is divided into three sections, is rectifying section more than the fresh solvent inlet, long 300mm is extraction section I between fresh solvent inlet and the recovery colvent inlet, long 500mm, reclaiming the colvent inlet is extraction section II at the bottom of tower, long 1150mm.The used filler of rectifying column is the stainless steel Dixon ring of Φ 3mm * 3mm.The body of the tower rock wool heat-preservation.
Measured the hydrodynamic parameters of system's discontinuous extracting rectifying system rectifying column before the experiment, determined that the rectifying column pressure drop in the normal running interval of experiment is 50～120mm water column, about about 500～1200Pa.Having measured Rectification Column's Theoretical Plate Number with benzene-carbon tetrachloride system at last is 46.With the mixture distillation of rectifying column with the second alcohol and water, the product that steams is the ethanol-water azeotropic thing of 95% (mass percent), with this raw material as experiment before experiment.
Experimental result and discussion
For feasibility that this experimental technique is described and than the superiority of conventional method, the result is analyzed from the following aspects.
1. the concentration of cat head extraction product
Beginning not have the solvent of recovery adding stage F
S=35ml/min; There is the solvent of recovery to add fashionable F
S=28ml/min, F
RS=17ml/min; Begin extraction after product design reaches 99.90%, carried out 4 extraction altogether, overhead fraction purity is up to 99.56%, and mean concentration is 99.37%.Illustrate and adopt this kind method can reach better products concentration.
2. solvent recovery situation
Table 1 solvent recovery still mode of operation
As can be seen from Table 1, this kind method of operating has been carried out 3 solvent recovery operations altogether in the operating process of batch fractionating, and glycol concentration about 80%, has organic efficiency preferably substantially in the recovery solvent.
In sum, for this system, it is fully feasible adopting this new manipulation method.
Claims (6)
1, a kind of double-kettle batch extraction rectification device of separating ethanol-water azeotropic system is characterized in that it mainly comprises: raw material still, solvent recovery still, intermediate storage tank, rectifying column, condenser, product jar, storage tank, valve; Solvent recovery still, intermediate storage tank, product jar and condenser are formed solvent recovery unit; Raw material still, product jar, condenser, valve are formed the batch fractionating device;
Connected mode: the raw material still is connected by intermediate storage tank with the solvent recovery still, be connected with triple valve in the middle of rectifying column, raw material still, the intermediate storage tank, top of tower is connected with condenser, is connected with trap on the condenser, and rectifying tower body and solvent recovery still all are connected with the product collecting tank; Two stills of described raw material still and solvent recovery still were connected with being connected by valve of rectifying column.
2, device according to claim 1 is characterized in that described rectifying column is the making of metal stainless steel, interior dress stainless steel Dixon ring filler.Rectifying column has fresh solvent inlet and recovery solvent to add inlet on one's body respectively, reclaims solvent and adds inlet below fresh solvent adds inlet.
3, device according to claim 2 is characterized in that it is 300mm apart from cat head that described fresh solvent adds inlet, reclaims solvent and adds inlet and add inlet apart from fresh solvent and be 550mm, apart from being 1150mm at the bottom of the tower.
4, device according to claim 1 is characterized in that described raw material still volume is 30L, and the solvent recovery still is 20L, all adopts heat-conducting oil heating.
5, device according to claim 1, the volume that it is characterized in that the product jar of described intermediate storage tank and solvent recovery still all is 10L.
6, the method for the described double-kettle batch extraction rectifying of claim 1 separating ethanol-water azeotropic system, its feature may further comprise the steps at it:
1) total reflux operation under the solvent-free adding
In the described raw material still of the disposable adding of alcohol-water raw material, close and connect solvent recovery system valve, open and connect batch fractionating system valve, make solvent recovery system and batch fractionating system isolated, in the batch fractionating system, carry out the normal pressure total reflux operation;
2) total reflux operation of fresh solvent under adding arranged
Total reflux operation adds inlet from the fresh solvent near cat head and adds fresh solvent after a period of stabilisation, and shut off valve this moment (8) is opened valve (9), makes the solvent of phegma and adding all enter intermediate storage tank, still carries out total reflux operation;
3) there is fresh solvent to decide the reflux ratio extraction under adding
In step 2) total reflux operation after a period of stabilisation, survey the concentration of cat head extraction product, reach after the extraction requirement with reflux ratio extraction in 1: 1, when the accumulation of fluid in the middle storage tank after to a certain degree, put it in the solvent recovery still; The solvent recovery still carries out simple distillation with bigger power heating, steams light component quickly, and the steam that is rich in light component enters the product jar of tower bottom after condenser condenses, and the liquid that remains in the solvent recovery jar is recovered solvent; This moment, the batch fractionating system still was in the stage of deciding the reflux ratio extraction;
4) total reflux operation under the solvent-free adding
When the temperature of solvent recovery still is elevated to uniform temperature, in the tower steam quantitative change seldom after, stop the heating of solvent recovery still.After this at first stop the adding of fresh solvent, with the liquid in the product jar, the disposable raw material still of putting into, valve-off is total reflux operation then;
5) fresh solvent and the total reflux operation of reclaiming under the solvent adding are arranged
Recovered solvent in the solvent recovery still is migrated out still, and constant temperature is in a certain temperature, and after infinite reflux was stable, shut off valve (9) was opened valve (8), and flow liquid is entered in the intermediate storage tank, and solvent after the recovery and fresh solvent add in the tower with certain speed respectively.The batch fractionating system is kept total reflux operation;
6) fresh solvent and reclaim solvent and decide the reflux ratio extraction under adding is arranged
After overhead fraction reaches qualified requirement, with certain reflux ratio extraction;
After this repeat 4), 5), 6) step, after cat head extraction product is defective, stops solvent and add, at last with the solvent recovery still, intermediate storage tank and recovered solvent add the raw material still and are recovered to high boiling solvent, this operating process so far finishes.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2007100601588A CN101279144A (en) | 2007-12-25 | 2007-12-25 | Double boiler intermittent extraction and rectification device for separating alcohol-water azeotropy system and method |
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| CNA2007100601588A CN101279144A (en) | 2007-12-25 | 2007-12-25 | Double boiler intermittent extraction and rectification device for separating alcohol-water azeotropy system and method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108992957A (en) * | 2018-09-29 | 2018-12-14 | 天津中福环保科技股份有限公司 | Recyclable device, skid structure and the method for multiple types solvent in a kind of dangerous waste process field |
| CN111530113A (en) * | 2020-05-07 | 2020-08-14 | 杭州制氧机集团股份有限公司 | Liquid distribution test system in large-scale packed tower and operation method |
-
2007
- 2007-12-25 CN CNA2007100601588A patent/CN101279144A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108992957A (en) * | 2018-09-29 | 2018-12-14 | 天津中福环保科技股份有限公司 | Recyclable device, skid structure and the method for multiple types solvent in a kind of dangerous waste process field |
| CN111530113A (en) * | 2020-05-07 | 2020-08-14 | 杭州制氧机集团股份有限公司 | Liquid distribution test system in large-scale packed tower and operation method |
| CN111530113B (en) * | 2020-05-07 | 2023-12-01 | 杭氧集团股份有限公司 | Liquid distribution test system in large-scale packed tower and operation method |
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