CN205347271U - Produce device of high straight alcohol - Google Patents
Produce device of high straight alcohol Download PDFInfo
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- CN205347271U CN205347271U CN201521132555.8U CN201521132555U CN205347271U CN 205347271 U CN205347271 U CN 205347271U CN 201521132555 U CN201521132555 U CN 201521132555U CN 205347271 U CN205347271 U CN 205347271U
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P20/10—Process efficiency
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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Abstract
The utility model relates to a produce device of high straight alcohol belongs to the chemical engineering technology field. Including low pressure rectifying column (2) and pressurized rectification tower (6), the top of the tower of low pressure rectifying column (2) export is connected with pressurized rectification tower (6), the top of the tower of pressurized rectification tower (6) export is connected with the entry of infiltration vaporization membrane (8), and the export of holding back the side that membrane (8) were vaporized in the infiltration is connected with molecular sieve adsorption tower (11). High straight alcohol is produced in two tower differential pressure rectification - membrane equipment - molecular sieve adsorption tower couplings, with traditional handicraft and novel stripping technique coupling, not limited by the azeotropy, need not add the third component, and the inside thermal coupling of system is the stripping technique of an energy -efficient environmental protection.
Description
Technical field
This utility model relates to a kind of device producing high straight alcohol, belongs to chemical technology field.
Background technology
High straight alcohol purposes is widely, for instance ultra-clean cleaning in the precise electronic components and parts course of processing, dry, the ultra-clean cleaning of Clean room apparatus, scientific experimentation, the important solvent of medication chemistry industry, but ethanol forms azeotropic mixture with water, adopts a kind of technology to be difficult to obtain high straight alcohol.
Current ethanol dehydration method mainly has rectification, azeotropic distillation and extracting rectifying can obtain anhydrous or that purity is higher ethanol, but both process energy consumptions are higher, all needs to add the 3rd component, also increases the environmental protection pressure of enterprise while increasing cost.Differential pressure rectification is a kind of novel energy-efficient distillation technology, utilize high-pressure tower tower top alcohol vapour to be condensed as the driving heat source of lower pressure column, having saved steam and condensed water, but differential pressure rectification is limited by azeotropic physical property, monotechnics can not obtain high-purity solvent.
Film dehydration technique utilize each component in separated liquid mixture dissolve in film (absorption) different from diffusion rate and realize separate, a kind of new separation technology, have energy-efficient, process is easily controllable, easy to operate, be easy to amplify and the advantage of industrialization.Along with the continuous progress of membrane material technology of preparing, application of membrane is developed rapidly.Its prominent advantage is that separation process is by the restriction of component vapor liquid equilibrium, it is possible to realize the task that the traditional methods such as rectification have been difficult to low energy consumption, such as azeotropic, closely boils the separation of mixture.But at present restriction film application mainly have following some: 1, the dehydration of high-moisture dicyandiamide solution is inapplicable, is affected by film production process, and film dehydration uses range feed water content≤30%, and the too high meeting of water content causes that film shortens service life；2, cost of investment, relative to the conventional art such as rectification, molecular sieve, membrane technology cost of investment is higher, and feed moisture content is higher or all can cause that membrane area increases to finished product purity requirement after film dehydration is too high, and this is also it is not recommended that utilize membrane technology to directly obtain the reason of high neat solvent.
Molecular sieve adsorption technology is the technique that current domestic and international application is wide, technology is more ripe, and dehydration is a physical process, will not cause environmental pollution and cause " three wastes " emission problem.Low concentration of water is still had significantly high adsorption efficiency by molecular sieve, and compared with and separation equipment dry with other, equipment investment is low.But this technology is not suitable for higher moisture solvent dehydration, reason be water content too high meeting when causing regenerating molecular sieve energy consumption significantly high, also result in molecular sieve, cause molecular sieve lattice disturbance, it is substantially reduced the adsorption efficiency of molecular sieve, molecular sieve powder may be brought in finished product, affects end product quality.Therefore adopt the feed moisture content general control≤6wt.% of molecular sieve adsorbing and dewatering.
Utility model content
The purpose of this utility model is to provide a kind of high-purity ethanol production process, two tower differential pressure rectification-tower-coupled high purity ethanol of film device-molecular sieve adsorption, traditional handicraft is coupled with new separation technology, do not limited by azeotropic, do not need to add the 3rd component, internal system thermal coupling, is the isolation technics of a kind of high-efficient energy-saving environment friendly.
A kind of technique producing high straight alcohol, comprises the steps:
1st step, sends into ethanol water and carries out rectification in low-pressure distillation tower, obtains the first overhead vapours and the first tower bottoms；Again the first overhead vapours is carried out rectification then through sending in compression rectification tower after condensation, obtain the second overhead vapours and the second tower bottoms；
2nd step, sends at least some of second overhead vapours in infiltrating and vaporizing membrane and carries out dehydration, obtain dewatered ethanol；
3rd step, then dewatered ethanol is carried out deep dehydration by the mode of molecular sieve adsorption, obtain high-purity alcohol vapour.
In the 1st described step, the concentration range 5～20wt% of ethanol water；Ethanol water, before entering low-pressure distillation tower, carries out heat exchange with the first tower bottoms and the first overhead vapours successively.
In the 1st described step, operating pressure preferable range 50～90kPa(absolute pressure of low-pressure distillation tower)；In compression rectification tower, working pressure range 250～500kPa(absolute pressure).
In the 1st described step, the first tower bottoms and high-purity alcohol vapour carry out heat exchange.
In the 2nd described step, some second overhead vapours and the first tower bottoms carry out after heat exchange again from the overhead reflux of compression rectification tower；And from the second overhead vapours of the overhead reflux of compression rectification tower with to enter the weight ratio of the second overhead vapours of infiltrating and vaporizing membrane be 1.5～3:1.
In the 2nd described step, the per-meate side of infiltrating and vaporizing membrane is negative-pressure operation, pressure limit 50～1500kPa；Infiltrating and vaporizing membrane is permeable molecular screen membrane, it is preferable that NaA film.
In the 3rd described step, molecular sieve adsorption operation pressure is 250～500kPa, operates temperature 130～150 DEG C；During regenerative operation, operation pressure is 50～80kPa, operates temperature 150～180 DEG C.
A kind of device producing high straight alcohol, includes low-pressure distillation tower and compression rectification tower, and the tower top outlet of low-pressure distillation tower is connected with compression rectification tower；The tower top outlet of compression rectification tower is connected with the entrance of infiltrating and vaporizing membrane, and the outlet retaining side of infiltrating and vaporizing membrane is connected with adsorbing tower with molecular sieve.
Low-pressure distillation tower is connected with feed conduit, and described mother tube exports with the tower reactor of low-pressure distillation tower and is connected for heat exchange between the tower top outlet of low-pressure distillation tower.
The tower top outlet of compression rectification tower also by and the tower reactor of low-pressure distillation tower between after heat exchange is connected, then be connected with the tower top of compression rectification tower.
The per-meate side of infiltrating and vaporizing membrane is connected with low-pressure distillation tower or compression rectification tower.
The outlet retaining side of infiltrating and vaporizing membrane is connected with adsorbing tower with molecular sieve by superheater again.
Infiltrating and vaporizing membrane is permeable molecular screen membrane, it is preferable that NaA film.
The outlet of adsorbing tower with molecular sieve carries out heat exchange with the tower reactor of low-pressure distillation tower again and is connected.
Beneficial effect
1, this utility model adopts two tower differential pressure rectification-tower-coupled high purity ethanol of film device-molecular sieve, is not limited by azeotropic, does not need to add the 3rd component, is the isolation technics of a kind of high-efficiency environment friendly.
2, this utility model only has compression rectification tower to need the external world to provide steam heating；Low-pressure distillation tower utilizes compression rectification column overhead steam and the heating of molecular sieve tower height straight alcohol steam.Compression rectification column overhead outlet gas phase is directly entered film device, and film device outlet gas phase is directly entered molecular sieve tower, and whole system internal heat recycles.Compared with traditional handicraft, energy-conservation more than 50%.
Accompanying drawing explanation
Fig. 1 is process chart schematic diagram；
1, preheater；2, low-pressure distillation tower；3, the first reboiler；4, the second reboiler；5, preheater；6, compression rectification tower；7, the 3rd reboiler；8, infiltrating and vaporizing membrane；9, pump；10, superheater；11, adsorbing tower with molecular sieve；12, condenser；13, vacuum pump.
Detailed description of the invention
Below by detailed description of the invention, this utility model is described in further detail.It will be apparent, however, to one skilled in the art, that the following example is merely to illustrate this utility model, and should not be regarded as limiting scope of the present utility model.Unreceipted concrete technology or condition person in embodiment, technology described by the document in this area or condition (" Chemical Engineering handbook " (second edition) that such as Shi Jun etc. write, Chemical Industry Press, 1996) or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, be can pass through city available from conventional products.
Approximate language used herein can be used for modifying the statement of any quantity in entire disclosure and claims, and it can be changed being not resulted in allowance when its relevant basic function changes.Therefore, such as term " about " value modified is not limited to specified exact value.In at least some cases, approximate language can be corresponding with the precision of the instrument for measuring this value.Unless indicated otherwise in context or statement, otherwise range limit can be combined and/or exchange, and this scope is confirmed as and includes all subranges contained herein.Except indicating in operation embodiment or elsewhere, the numeral of the amount of all expression compositions that uses in specification and claims, reaction condition etc. or express and shall be construed as the modification being subject to word " about " in all cases.
In this utility model, term " heat exchange connection " refers to the connected mode of a kind of pipeline and pipeline, feed liquid between pipeline and pipeline is not be interconnected, and referring to that the outer wall of these two pipelines is connected with each other the mixing that can exchange heat each other and be unlikely to make feed liquid, this connected mode generally can be through heat exchanger and is connected with each other.Heat exchanger can be chosen according to practical situation, it does not have limits especially, it is possible to enumerates: pipe heat exchanger, plate type heat exchanger, finned heat exchanger, heat exchange of heat pipe etc..
The aquiferous ethanol raw material that this utility model is suitable for may refer to the recovery ethanol in synthetic reaction, it is also possible to refers to the aquiferous ethanol in industrial process, also can be suitably used for the fermentation liquid containing ethanol obtained in fermentation legal system ethanol.For the ethanol as solvent in synthetic reaction, raw material, impurity etc. that a certain amount of unreacted completes wherein also can be contained；And for fermentation liquid, a certain amount of sulfur wherein can be contained, the total amount being usually the compound with sulfur-bearing contained in fermentation liquid raw material represents.The aqueous solution of fermenting alcohol can remove big insoluble composition by coarse filtration before input rectifying column.
High-purity ethanol production process that this utility model provides, two tower differential pressure rectification-tower-coupled high purity ethanol of film device-molecular sieve adsorption, traditional handicraft is coupled with new separation technology, is not limited by azeotropic, do not need to add the 3rd component, internal system thermal coupling.Wherein, two rectifying columns refer to low-pressure distillation tower and high-pressure rectification tower, low-pressure distillation tower outside need not be additionally provided heat, simply use other waste heat in system, it can make ethanol water obtain preliminary separation, the overhead vapours of its generation is re-fed in compression rectification tower to carry out the separation of rectification further, and the overhead vapours of generation passes sequentially through the method for infiltrating and vaporizing membrane and molecular sieve adsorption again and carries out deep dehydration, can realize the preparation of highly purified ethanol.
The ethanol water as raw material that this utility model adopts, the concentration range of ethanol therein can be at 5～20wt%, the waste heat simply using in system to make low-pressure distillation tower not need external world's offer additional heat, feed ethanol aqueous solution is when entering low-pressure distillation tower, it is possible to first preheat with the tower bottoms of low-pressure distillation tower, low-pressure distillation tower overhead vapours (the first overhead vapours) successively；Feed entrance point is preferably the middle and upper part of low-pressure distillation tower.Operating pressure preferable range 50～90kPa(absolute pressure of low-pressure distillation tower), low-pressure distillation tower overhead vapours is then through, after condensation, sending in compression rectification tower and be additionally separated.
In compression rectification tower, operating pressure preferable range 250～500kPa(absolute pressure), tower top at compression rectification tower obtains moisture 10～25wt.% ethanol malleation steam (the second overhead vapours), this steam is divided into two strands, after wherein one tower bottoms with low-pressure distillation tower carries out heat exchange, returning again to the overhead reflux to compression rectification tower, another burst of gas phase is directly entered follow-up oozes vaporization film device, has not only purified film raw material but also saved the energy again vaporized；The overhead extraction of compression rectification tower can be 1.5～3:1 for the azeotropic ethanol steam of low-pressure distillation tower heat supply with entering film alcohol vapour mass ratio.
Come from after the steam of the tower top of compression rectification tower is directly entered infiltrating and vaporizing membrane, carry out osmotic, evaporating and dewatering, film equipment per-meate side negative-pressure operation, its operation pressure is 50～1500kPa(absolute pressure), operation temperature is the temperature overheating 10～20 DEG C that system saturated vapor pressure is corresponding；Infiltrating and vaporizing membrane is equipped for permeable molecular screen membrane, it is preferable that NaA film；Ethanol malleation steam enters film equipment, separates through membrane module, and the alcohol vapour that film outlet (positive pressure side) is moisture 1000～5000ppm, suction side is the aqueous solution containing a small amount of ethanol.
Dewatered ethanol in infiltrating and vaporizing membrane film is re-fed into follow-up molecular sieve tower and carries out deep dehydration, and the operation pressure of molecular sieve tower is 250～500kPa, operates temperature 130～150 DEG C；The operation pressure of regenerator is 50～80kPa, operates temperature 150～180 DEG C, it is thus achieved that the high straight alcohol of moisture 50～100ppm, and high-purity alcohol vapour, for the reboiler of low-pressure distillation tower is heated, makes full use of waste heat.
The Diluted Alcohol that infiltration evaporation film device suction side penetrating fluid and regenerating molecular sieve obtain may return to low pressure or compression rectification tower reclaims.
In 2 rectifying columns, only compression rectification tower needs the external world to provide steam heating；Low-pressure distillation tower utilizes overhead vapours and the heating of molecular sieve tower height straight alcohol steam of compression rectification tower.
Based on above-mentioned method, the device that this utility model adopts structure as shown in Figure 1, include low-pressure distillation tower 2 and compression rectification tower 6, the tower top outlet of low-pressure distillation tower 2 is connected with compression rectification tower 6；The tower top outlet of compression rectification tower 6 is connected with the entrance of infiltrating and vaporizing membrane 8, and the outlet retaining side of infiltrating and vaporizing membrane 8 is connected with adsorbing tower with molecular sieve 11.
Low-pressure distillation tower 2 is connected with feed conduit, and described mother tube exports with the tower reactor of low-pressure distillation tower 2 and is connected for heat exchange between the tower top outlet of low-pressure distillation tower 2.Its effect is to realize the heat exchange between tower reactor feed liquid and the overhead vapours of feed ethanol solution and low-pressure distillation tower 2, it is achieved the preheating of raw material.
The tower top outlet of compression rectification tower 6 is also by after being connected with heat exchange between the tower reactor of low-pressure distillation tower 2, then is connected with the tower top of compression rectification tower 6.Its effect is to realize the overhead vapours heat exchange of compression rectification tower 6 to low-pressure distillation tower 2, and the steam of condensation can also be formed the backflow of compression rectification tower 6 simultaneously.
The per-meate side of infiltrating and vaporizing membrane 8 is connected with low-pressure distillation tower 2 or compression rectification tower 6.Purpose is to realize the reuse of the infiltration evaporation permeate containing a certain amount of ethanol.The regenerated liquid outlet of adsorbing tower with molecular sieve 11 is connected with low-pressure distillation tower 2 or compression rectification tower 6.Purpose is to realize the reuse of the regenerated liquid containing a certain amount of ethanol.
The outlet retaining side of infiltrating and vaporizing membrane 8 is connected with adsorbing tower with molecular sieve 11 by superheater 10 again.Its effect is the hot feed excessively realizing dehydration steam.
The outlet of adsorbing tower with molecular sieve 11 carries out heat exchange with the tower reactor of low-pressure distillation tower 2 again and is connected.Its objective is to realize UTILIZATION OF VESIDUAL HEAT IN and the condensation of the dewatered ethanol steam of high temperature.
Embodiment 1
As shown in Figure 1, the low-concentration ethanol mother solution of ethanol content 20wt.% is through the tower bottoms of low-pressure distillation tower 2, the top of low-pressure distillation tower 2 is entered after tower top raw distillate stream steam preheating, after rectification, tower reactor obtains still residual liquid, tower top obtains the steam of ethanol content 50wt.%, steam is for preheating raw material, steam after preheating material enters compression rectification tower 6, after rectification, tower reactor obtains the waste water of ethanol content≤0.1wt.%, tower top obtains ethanol content 80wt.% malleation stream vapor, malleation ethanol stream is divided into two strands, returning the compression rectification tower mass ratio with two strands that enter infiltrating and vaporizing membrane is 2:1, as compression rectification tower 6 backflow after the plume of return compression rectification tower and the tower reactor reboiler heat exchange condensation of low-pressure distillation tower 2, the gas phase extraction entering infiltrating and vaporizing membrane enters permeable molecular screen membrane equipment (NaA molecular sieve membrane), evacuation is surveyed in molecular screen membrane equipment infiltration, form feed side poor with osmotic lateral pressure, power is provided by film for steam.It is divided into, through permeable molecular screen membrane equipment, the dewatered ethanol and penetrating fluid that retain side, after penetrating fluid (water content >=95wt.%) condensation, is back to front workshop section, as low-pressure distillation tower 2 raw material, reclaim ethanol a small amount of in penetrating fluid, improve yield.The dewatered ethanol retaining side is 99.5wt.% ethanol crude product malleation steam, if it is different from adsorbing tower with molecular sieve operation pressure to enter adsorbing tower with molecular sieve 11(film equipment after this malleation steam superheating, heat pump need to be increased, after heat after compression on pipeline), obtain 99.99% high-purity alcohol vapour.Adsorbing tower with molecular sieve is Petronas Towers, two tower absorption regeneration handover operations, and the Diluted Alcohol (water content is about 5wt.%) that regeneration produces also returns to low-pressure distillation tower 2.High-purity alcohol vapour, for low-pressure distillation tower 2 reboiler is heated, makes full use of waste heat.Whole workshop section only has low-pressure distillation tower 2 and compression rectification tower 6 still residual liquid discharge port, ethanol content≤0.1wt.%.
Main operating parameters condition is as follows: producing 40000 tons of 99.99wt.% ethanol per year, low-pressure distillation tower 2 number of plates is 28, and the feed entrance point of raw material is the 3rd block of column plate, operation pressure is 80kPa, tower top temperature 75 DEG C, bottom temperature 95 DEG C, the mass flow of overhead vapours is 11.2t/h；Compression rectification tower 6 number of plates is 38, and feed entrance point is the 31st block of column plate, and operation pressure is 380kPa, tower top temperature 115 DEG C, bottom temperature 135 DEG C, and the overhead vapours mass flow entering infiltrating and vaporizing membrane 8 is 6.95t/h.Infiltrating and vaporizing membrane 8 feed side operation pressure is 340kPa, operates temperature 130 DEG C, and per-meate side operation pressure is 1200Pa, and membrance separation unit is in series by 10 membrane modules, and film average flux is 1.80kg/m2H, the mass flow of membrane permeation liquid is 1.42t/h, and it is 5.53t/h that the infiltrating and vaporizing membrane 8 of entrance adsorbing tower with molecular sieve 11 retains side dewatered ethanol mass flow, and molecular sieve tower operation pressure is 300kPa, operation temperature 140 DEG C, the high-purity alcohol vapour mass flow of adsorbing tower with molecular sieve 11 is 5t/h.Producing 1 ton of 99.99% ethanol needs consumption quantity of steam to be 2.0 tons.
Embodiment 2
As shown in Figure 1, the low-concentration ethanol mother solution of ethanol content 25wt.% is through the tower bottoms of low-pressure distillation tower 2, the top of low-pressure distillation tower 2 is entered after tower top raw distillate stream steam preheating, after rectification, tower reactor obtains still residual liquid, tower top obtains the steam of ethanol content 57wt.%, steam is for preheating raw material, steam after preheating material enters compression rectification tower 6, after rectification, tower reactor obtains the waste water of ethanol content≤0.1wt.%, tower top obtains ethanol content 85wt.% malleation stream vapor, malleation ethanol stream is divided into two strands, returning the compression rectification tower mass ratio with two strands that enter infiltrating and vaporizing membrane is 3:1, as compression rectification tower 6 backflow after the plume of return compression rectification tower and the tower reactor reboiler heat exchange condensation of low-pressure distillation tower 2, the gas phase extraction entering infiltrating and vaporizing membrane enters permeable molecular screen membrane equipment (NaA molecular sieve membrane), evacuation is surveyed in molecular screen membrane equipment infiltration, form feed side poor with osmotic lateral pressure, power is provided by film for steam.It is divided into, through permeable molecular screen membrane equipment, the dewatered ethanol and penetrating fluid that retain side, after penetrating fluid (water content >=95wt.%) condensation, is back to front workshop section, as low-pressure distillation tower 2 raw material, reclaim ethanol a small amount of in penetrating fluid, improve yield.The dewatered ethanol retaining side is 99.1wt.% ethanol crude product malleation steam, if it is different from adsorbing tower with molecular sieve operation pressure to enter adsorbing tower with molecular sieve 11(film equipment after this malleation steam superheating, heat pump need to be increased, after heat after compression on pipeline), obtain 99.99% high-purity alcohol vapour.Adsorbing tower with molecular sieve is Petronas Towers, two tower absorption regeneration handover operations, and the Diluted Alcohol (water content is about 7wt.%) that regeneration produces also returns to low-pressure distillation tower 2.High-purity alcohol vapour, for low-pressure distillation tower 2 reboiler is heated, makes full use of waste heat.Whole workshop section only has low-pressure distillation tower 2 and compression rectification tower 6 still residual liquid discharge port, ethanol content≤0.1wt.%.
Main operating parameters condition is as follows: producing 40000 tons of 99.99wt.% ethanol per year, low-pressure distillation tower 2 number of plates is 25, and the feed entrance point of raw material is the 4th block of column plate, operation pressure is 120kPa, tower top temperature 70 DEG C, bottom temperature 90 DEG C, the mass flow of overhead vapours is 10.3t/h；Compression rectification tower 6 number of plates is 33, and feed entrance point is the 27th block of column plate, and operation pressure is 420kPa, tower top temperature 125 DEG C, bottom temperature 125 DEG C, and the overhead vapours mass flow entering infiltrating and vaporizing membrane 8 is 6.55t/h.Infiltrating and vaporizing membrane 8 feed side operation pressure is 330kPa, operates temperature 120 DEG C, and per-meate side operation pressure is 1100Pa, and membrance separation unit is in series by 12 membrane modules, and film average flux is 1.70kg/m2H, the mass flow of membrane permeation liquid is 1.24t/h, and it is 5.31t/h that the infiltrating and vaporizing membrane 8 of entrance adsorbing tower with molecular sieve 11 retains side dewatered ethanol mass flow, and molecular sieve tower operation pressure is 320kPa, operation temperature 130 DEG C, the high-purity alcohol vapour mass flow of adsorbing tower with molecular sieve 11 is 5t/h.Producing 1 ton of 99.99% ethanol needs consumption quantity of steam to be 2.2 tons.
Embodiment 3
It is distinctive in that with embodiment 2: the penetrating fluid of infiltrating and vaporizing membrane 8 can also return compression rectification tower 6 and carry out charging.
As shown in Figure 1, the low-concentration ethanol mother solution of ethanol content 25wt.% is through the tower bottoms of low-pressure distillation tower 2, the top of low-pressure distillation tower 2 is entered after tower top raw distillate stream steam preheating, after rectification, tower reactor obtains still residual liquid, tower top obtains the steam of ethanol content 62wt.%, steam is for preheating raw material, steam after preheating material enters compression rectification tower 6, after rectification, tower reactor obtains the waste water of ethanol content≤0.1wt.%, tower top obtains ethanol content 87wt.% malleation stream vapor, malleation ethanol stream is divided into two strands, returning the compression rectification tower mass ratio with two strands that enter infiltrating and vaporizing membrane is 3:1, as compression rectification tower 6 backflow after the plume of return compression rectification tower and the tower reactor reboiler heat exchange condensation of low-pressure distillation tower 2, the gas phase extraction entering infiltrating and vaporizing membrane enters permeable molecular screen membrane equipment (NaA molecular sieve membrane), evacuation is surveyed in molecular screen membrane equipment infiltration, form feed side poor with osmotic lateral pressure, power is provided by film for steam.It is divided into, through permeable molecular screen membrane equipment, the dewatered ethanol and penetrating fluid that retain side, after penetrating fluid (water content >=95wt.%) condensation, is back to front workshop section, as compression rectification tower 6 raw material, reclaim ethanol a small amount of in penetrating fluid, improve yield.The dewatered ethanol retaining side is 99.3wt.% ethanol crude product malleation steam, if it is different from adsorbing tower with molecular sieve operation pressure to enter adsorbing tower with molecular sieve 11(film equipment after this malleation steam superheating, heat pump need to be increased, after heat after compression on pipeline), obtain 99.99% high-purity alcohol vapour.Adsorbing tower with molecular sieve is Petronas Towers, two tower absorption regeneration handover operations, and the Diluted Alcohol (water content is about 7wt.%) that regeneration produces also returns to low-pressure distillation tower 2.High-purity alcohol vapour, for low-pressure distillation tower 2 reboiler is heated, makes full use of waste heat.Whole workshop section only has low-pressure distillation tower 2 and compression rectification tower 6 still residual liquid discharge port, ethanol content≤0.1wt.%.
Main operating parameters condition is as follows: producing 40000 tons of 99.99wt.% ethanol per year, low-pressure distillation tower 2 number of plates is 25, and the feed entrance point of raw material is the 4th block of column plate, operation pressure is 120kPa, tower top temperature 70 DEG C, bottom temperature 90 DEG C, the mass flow of overhead vapours is 10.2t/h；Compression rectification tower 6 number of plates is 33, and feed entrance point is the 27th block of column plate, and operation pressure is 420kPa, tower top temperature 125 DEG C, bottom temperature 125 DEG C, and the overhead vapours mass flow entering infiltrating and vaporizing membrane 8 is 6.95t/h.Infiltrating and vaporizing membrane 8 feed side operation pressure is 330kPa, operates temperature 120 DEG C, and per-meate side operation pressure is 1100Pa, and membrance separation unit is in series by 12 membrane modules, and film average flux is 1.97kg/m2H, the mass flow of membrane permeation liquid is 1.18t/h, and it is 5.77t/h that the infiltrating and vaporizing membrane 8 of entrance adsorbing tower with molecular sieve 11 retains side dewatered ethanol mass flow, and molecular sieve tower operation pressure is 320kPa, operation temperature 130 DEG C, the high-purity alcohol vapour mass flow of adsorbing tower with molecular sieve 11 is 5.2t/h.Producing 1 ton of 99.99% ethanol needs consumption quantity of steam to be 2.0 tons.
Embodiment 4
As shown in Figure 1, the low-concentration ethanol mother solution of ethanol content 22wt.% is through the tower bottoms of low-pressure distillation tower 2, the top of low-pressure distillation tower 2 is entered after tower top raw distillate stream steam preheating, after rectification, tower reactor obtains still residual liquid, tower top obtains the steam of ethanol content 51wt.%, steam is for preheating raw material, steam after preheating material enters compression rectification tower 6, after rectification, tower reactor obtains the waste water of ethanol content≤0.1wt.%, tower top obtains ethanol content 85wt.% malleation stream vapor, malleation ethanol stream is divided into two strands, returning the compression rectification tower mass ratio with two strands that enter infiltrating and vaporizing membrane is 2:1, as compression rectification tower 6 backflow after the plume of return compression rectification tower and the tower reactor reboiler heat exchange condensation of low-pressure distillation tower 2, the gas phase extraction entering infiltrating and vaporizing membrane enters permeable molecular screen membrane equipment (NaA molecular sieve membrane), evacuation is surveyed in molecular screen membrane equipment infiltration, form feed side poor with osmotic lateral pressure, power is provided by film for steam.It is divided into, through permeable molecular screen membrane equipment, the dewatered ethanol and penetrating fluid that retain side, after penetrating fluid (water content >=95wt.%) condensation, is back to front workshop section, as low-pressure distillation tower 2 raw material, reclaim ethanol a small amount of in penetrating fluid, improve yield.The dewatered ethanol retaining side is 99.3wt.% ethanol crude product malleation steam, if it is different from adsorbing tower with molecular sieve operation pressure to enter adsorbing tower with molecular sieve 11(film equipment after this malleation steam superheating, heat pump need to be increased, after heat after compression on pipeline), obtain 99.99% high-purity alcohol vapour.Adsorbing tower with molecular sieve is Petronas Towers, two tower absorption regeneration handover operations, and the Diluted Alcohol (water content is about 6wt.%) that regeneration produces also returns to low-pressure distillation tower 2.High-purity alcohol vapour, for low-pressure distillation tower 2 reboiler is heated, makes full use of waste heat.Whole workshop section only has low-pressure distillation tower 2 and compression rectification tower 6 still residual liquid discharge port, ethanol content≤0.1wt.%.
Main operating parameters condition is as follows: producing 40000 tons of 99.99wt.% ethanol per year, low-pressure distillation tower 2 number of plates is 20, and the feed entrance point of raw material is the 6th block of column plate, operation pressure is 110kPa, tower top temperature 75 DEG C, bottom temperature 95 DEG C, the mass flow of overhead vapours is 11.5t/h；Compression rectification tower 6 number of plates is 40, and feed entrance point is the 22nd block of column plate, and operation pressure is 400kPa, tower top temperature 120 DEG C, bottom temperature 135 DEG C, and the overhead vapours mass flow entering infiltrating and vaporizing membrane 8 is 6.25t/h.Infiltrating and vaporizing membrane 8 feed side operation pressure is 310kPa, operates temperature 125 DEG C, and per-meate side operation pressure is 1400Pa, and membrance separation unit is in series by 10 membrane modules, and film average flux is 1.75kg/m2H, the mass flow of membrane permeation liquid is 1.20t/h, and it is 5.05t/h that the infiltrating and vaporizing membrane 8 of entrance adsorbing tower with molecular sieve 11 retains side dewatered ethanol mass flow, and molecular sieve tower operation pressure is 300kPa, operation temperature 120 DEG C, the high-purity alcohol vapour mass flow of adsorbing tower with molecular sieve 11 is 4.9t/h.Producing 1 ton of 99.99% ethanol needs consumption quantity of steam to be 2.2 tons.
Embodiment 5
The present embodiment adopts the alcoholic solution that biomass ferment method obtains, and fermentation liquid first passes through coarse filter and ceramic membrane filter remove impurity in advance.As shown in Figure 1, the low-concentration ethanol mother solution of ethanol content 8wt.% is (possibly together with propanol 300ppm, methanol 100ppm, sulfide compound 30ppm etc.) through the tower bottoms of low-pressure distillation tower 2, the top of low-pressure distillation tower 2 is entered after tower top raw distillate stream steam preheating, after rectification, tower reactor obtains still residual liquid, tower top obtains the steam of ethanol content 34wt.%, steam is for preheating raw material, steam after preheating material enters compression rectification tower 6, after rectification, tower reactor obtains the waste water of ethanol content≤0.1wt.%, tower top obtains ethanol content 64wt.% malleation stream vapor, malleation ethanol stream is divided into two strands, returning the compression rectification tower mass ratio with two strands that enter infiltrating and vaporizing membrane is 2:1, as compression rectification tower 6 backflow after the plume of return compression rectification tower and the tower reactor reboiler heat exchange condensation of low-pressure distillation tower 2, the gas phase extraction entering infiltrating and vaporizing membrane enters permeable molecular screen membrane equipment (NaA molecular sieve membrane), evacuation is surveyed in molecular screen membrane equipment infiltration, form feed side poor with osmotic lateral pressure, power is provided by film for steam.It is divided into, through permeable molecular screen membrane equipment, the dewatered ethanol and penetrating fluid that retain side, after penetrating fluid (water content 94wt.%, sulphur compound 140ppm) condensation, is back to front workshop section, as low-pressure distillation tower 2 raw material, reclaim ethanol a small amount of in penetrating fluid, improve yield.The dewatered ethanol retaining side is 98.1wt.% ethanol crude product malleation steam, if it is different from adsorbing tower with molecular sieve operation pressure to enter adsorbing tower with molecular sieve 11(film equipment after this malleation steam superheating, heat pump need to be increased, after heat after compression on pipeline), obtain 99.7% high-purity alcohol vapour.Adsorbing tower with molecular sieve is Petronas Towers, two tower absorption regeneration handover operations, and the Diluted Alcohol (water content is about 4wt.%) that regeneration produces also returns to low-pressure distillation tower 2.High-purity alcohol vapour, for low-pressure distillation tower 2 reboiler is heated, makes full use of waste heat.Whole workshop section only has low-pressure distillation tower 2 and compression rectification tower 6 still residual liquid discharge port, ethanol content≤0.1wt.%.
Main operating parameters condition is as follows: producing 40000 tons of 99.7wt.% ethanol per year, low-pressure distillation tower 2 number of plates is 22, and the feed entrance point of raw material is the 5th block of column plate, operation pressure is 130kPa, tower top temperature 65 DEG C, bottom temperature 95 DEG C, the mass flow of overhead vapours is 11.4t/h；Compression rectification tower 6 number of plates is 31, and feed entrance point is the 24th block of column plate, and operation pressure is 350kPa, tower top temperature 120 DEG C, bottom temperature 135 DEG C, and the overhead vapours mass flow entering infiltrating and vaporizing membrane 8 is 6.25t/h.Infiltrating and vaporizing membrane 8 feed side operation pressure is 340kPa, operates temperature 110 DEG C, and per-meate side operation pressure is 1000Pa, and membrance separation unit is in series by 14 membrane modules, and film average flux is 1.65kg/m2H, the mass flow of membrane permeation liquid is 1.35t/h, and it is 4.9t/h that the infiltrating and vaporizing membrane 8 of entrance adsorbing tower with molecular sieve 11 retains side dewatered ethanol mass flow, and molecular sieve tower operation pressure is 330kPa, operation temperature 125 DEG C, the high-purity alcohol vapour mass flow of adsorbing tower with molecular sieve 11 is 5t/h.Producing 1 ton of 99.7% ethanol needs consumption quantity of steam to be 2.2 tons.
Embodiment 6
The present embodiment adopts the alcoholic solution that biomass ferment method obtains, and fermentation liquid first passes through coarse filter and ceramic membrane filter remove impurity in advance.As shown in Figure 1, the low-concentration ethanol mother solution of ethanol content 8wt.% is (possibly together with propanol 300ppm, methanol 100ppm, sulfide compound 30ppm etc.) through the tower bottoms of low-pressure distillation tower 2, the top of low-pressure distillation tower 2 is entered after tower top raw distillate stream steam preheating, after rectification, tower reactor obtains still residual liquid, tower top obtains the steam of ethanol content 34wt.%, steam is for preheating raw material, steam after preheating material enters compression rectification tower 6, after rectification, tower reactor obtains the waste water of ethanol content≤0.1wt.%, tower top obtains ethanol content 64wt.% malleation stream vapor, malleation ethanol stream is divided into two strands, returning the compression rectification tower mass ratio with two strands that enter infiltrating and vaporizing membrane is 2:1, as compression rectification tower 6 backflow after the plume of return compression rectification tower and the tower reactor reboiler heat exchange condensation of low-pressure distillation tower 2, the gas phase extraction entering infiltrating and vaporizing membrane enters permeable molecular screen membrane equipment (NaA molecular sieve membrane), evacuation is surveyed in molecular screen membrane equipment infiltration, form feed side poor with osmotic lateral pressure, power is provided by film for steam.It is divided into, through permeable molecular screen membrane equipment, the dewatered ethanol and penetrating fluid that retain side, after penetrating fluid (water content 94wt.%, sulphur compound 140ppm) condensation, adds O3It is back to front workshop section after carrying out oxidation processes, as low-pressure distillation tower 2 raw material, reclaims ethanol a small amount of in penetrating fluid, improve yield.The dewatered ethanol retaining side is 98.4wt.% ethanol crude product malleation steam, if it is different from adsorbing tower with molecular sieve operation pressure to enter adsorbing tower with molecular sieve 11(film equipment after this malleation steam superheating, heat pump need to be increased, after heat after compression on pipeline), obtain 99.8% high-purity alcohol vapour.Adsorbing tower with molecular sieve is Petronas Towers, two tower absorption regeneration handover operations, and the Diluted Alcohol (water content is about 4wt.%) that regeneration produces also returns to low-pressure distillation tower 2.High-purity alcohol vapour, for low-pressure distillation tower 2 reboiler is heated, makes full use of waste heat.Whole workshop section only has low-pressure distillation tower 2 and compression rectification tower 6 still residual liquid discharge port, ethanol content≤0.1wt.%.
Main operating parameters condition is as follows: producing 40000 tons of 99.8wt.% ethanol per year, low-pressure distillation tower 2 number of plates is 22, and the feed entrance point of raw material is the 5th block of column plate, operation pressure is 130kPa, tower top temperature 65 DEG C, bottom temperature 95 DEG C, the mass flow of overhead vapours is 11.4t/h；Compression rectification tower 6 number of plates is 31, and feed entrance point is the 24th block of column plate, and operation pressure is 350kPa, tower top temperature 120 DEG C, bottom temperature 135 DEG C, and the overhead vapours mass flow entering infiltrating and vaporizing membrane 8 is 6.25t/h.Infiltrating and vaporizing membrane 8 feed side operation pressure is 340kPa, operates temperature 110 DEG C, and per-meate side operation pressure is 1000Pa, and membrance separation unit is in series by 14 membrane modules, and film average flux is 1.75kg/m2H, the mass flow of membrane permeation liquid is 1.35t/h, and it is 4.9t/h that the infiltrating and vaporizing membrane 8 of entrance adsorbing tower with molecular sieve 11 retains side dewatered ethanol mass flow, and molecular sieve tower operation pressure is 330kPa, operation temperature 125 DEG C, the high-purity alcohol vapour mass flow of adsorbing tower with molecular sieve 11 is 5t/h.Producing 1 ton of 99.7% ethanol needs consumption quantity of steam to be 2.0 tons.
Claims (8)
1. produce a device for high straight alcohol, include low-pressure distillation tower (2) and compression rectification tower (6), it is characterised in that: the tower top outlet of low-pressure distillation tower (2) is connected with compression rectification tower (6)；The tower top outlet of compression rectification tower (6) is connected with the entrance of infiltrating and vaporizing membrane (8), and the outlet retaining side of infiltrating and vaporizing membrane (8) is connected with adsorbing tower with molecular sieve (11).
2. the device of the high straight alcohol of production according to claim 1, it is characterized in that: low-pressure distillation tower (2) is connected with feed conduit, described mother tube exports with the tower reactor of low-pressure distillation tower (2) and is connected for heat exchange between the tower top outlet of low-pressure distillation tower (2).
3. the device of the high straight alcohol of production according to claim 1, it is characterised in that: the tower top outlet of compression rectification tower (6) is also by after being connected with heat exchange between the tower reactor of low-pressure distillation tower (2), then is connected with the tower top of compression rectification tower (6).
4. the device of the high straight alcohol of production according to claim 1, it is characterised in that: the per-meate side of infiltrating and vaporizing membrane (8) is connected with low-pressure distillation tower (2) or compression rectification tower (6).
5. the device of the high straight alcohol of production according to claim 1, it is characterised in that: the outlet retaining side of infiltrating and vaporizing membrane (8) is connected with adsorbing tower with molecular sieve (11) by superheater (10) again.
6. the device of the high straight alcohol of production according to claim 1, it is characterised in that: infiltrating and vaporizing membrane (8) is permeable molecular screen membrane.
7. the device of the high straight alcohol of production according to claim 6, it is characterised in that: described permeable molecular screen membrane is NaA film.
8. the device of the high straight alcohol of production according to claim 1, it is characterised in that: the outlet of adsorbing tower with molecular sieve (11) carries out heat exchange with the tower reactor of low-pressure distillation tower (2) again and is connected.
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| CN112194567A (en) * | 2020-11-03 | 2021-01-08 | 山东中盛药化设备有限公司 | Process and system for recovering absolute ethyl alcohol by combining rectification, vaporization membrane and MVR (mechanical vapor recompression) technology |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112194567A (en) * | 2020-11-03 | 2021-01-08 | 山东中盛药化设备有限公司 | Process and system for recovering absolute ethyl alcohol by combining rectification, vaporization membrane and MVR (mechanical vapor recompression) technology |
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