CN211078979U - Device for producing fuel ethanol and electronic grade ethanol - Google Patents
Device for producing fuel ethanol and electronic grade ethanol Download PDFInfo
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- CN211078979U CN211078979U CN201922009606.2U CN201922009606U CN211078979U CN 211078979 U CN211078979 U CN 211078979U CN 201922009606 U CN201922009606 U CN 201922009606U CN 211078979 U CN211078979 U CN 211078979U
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 307
- 239000000446 fuel Substances 0.000 title claims abstract description 40
- 239000012528 membrane Substances 0.000 claims abstract description 129
- 238000002242 deionisation method Methods 0.000 claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000004821 distillation Methods 0.000 claims description 66
- 238000000926 separation method Methods 0.000 claims description 41
- 239000002808 molecular sieve Substances 0.000 claims description 27
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 27
- 238000001728 nano-filtration Methods 0.000 claims description 11
- 239000012510 hollow fiber Substances 0.000 claims description 8
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 239000003014 ion exchange membrane Substances 0.000 claims description 3
- -1 feedstock pump (1) Chemical compound 0.000 claims description 2
- 230000000712 assembly Effects 0.000 claims 1
- 238000000429 assembly Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 10
- 230000006978 adaptation Effects 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 description 87
- 229960004756 ethanol Drugs 0.000 description 71
- 239000007788 liquid Substances 0.000 description 16
- 239000002699 waste material Substances 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 9
- 238000001914 filtration Methods 0.000 description 9
- 230000018044 dehydration Effects 0.000 description 8
- 238000006297 dehydration reaction Methods 0.000 description 8
- 238000000855 fermentation Methods 0.000 description 5
- 230000004151 fermentation Effects 0.000 description 5
- 239000001760 fusel oil Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 230000008878 coupling Effects 0.000 description 4
- 238000010168 coupling process Methods 0.000 description 4
- 238000005859 coupling reaction Methods 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 230000008595 infiltration Effects 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 238000005371 permeation separation Methods 0.000 description 3
- 238000005373 pervaporation Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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Abstract
The utility model relates to an ethanol production field specifically discloses a device of production fuel ethanol, electronic grade ethanol. The device includes raw material pump (1), mash preheater (2), gas retort (3), gas retort top condenser (4), gas retort bottom reboiler (5), I rectifying column (6), I rectifying column top condenser (7), reboiler (8) at the bottom of I rectifying column, flash drum (9), II rectifying column (10), II rectifying column top condenser (11), reboiler (12) at the bottom of II rectifying column, vapor permeable membrane separator (13), condensing tank (14), deionization membrane device (15), can produce two kinds of products of fuel ethanol and electronic grade ethanol simultaneously, the demand of adaptation market pluralism. In addition, the surplus heat energy of the device can be effectively utilized, the energy is fully matched and utilized, the steam consumption is saved, and compared with the traditional process, the steam can be saved by more than 20%.
Description
Technical Field
The utility model relates to an ethanol production field specifically relates to a device of production fuel ethanol, electronic grade ethanol.
Background
With the continuous development of electronic technology, the cleaning problem of precise electronic components and chips is more and more concerned. The ultra-clean high-purity chemical reagent is mainly used for solving the problems, wherein electronic grade absolute ethyl alcohol is taken as one of ultra-clean high-purity chemicals and is widely applied to various fields of military industry, chemical industry, electronics, energy, machinery, environmental protection, medicine and the like at present. Because the electronic grade ethanol has high quality requirement, has strict requirement on production environment and cannot be widely produced. The common purification technologies include distillation, rectification, reduced pressure distillation, gas absorption and the like, and the purification technologies have characteristics of large equipment investment and high energy consumption, so that the purification technologies are not widely applied. Under the condition of increasingly scarce resources, a new process for producing electronic-grade ethanol with low energy consumption is urgently needed. Chinese patent CN102260140A proposes that gases near azeotropic composition at the top of a rectifying tower are all condensed into liquid, then the liquid is heated to 80-90 ℃ and then sent into an infiltration vaporization membrane component, which causes huge waste of energy consumption, and simultaneously, serious concentration polarization and temperature difference polarization phenomena are generated in the liquid infiltration vaporization process. Chinese patent CN206980234U proposes a filtering device for specific electronic grade ethanol, but the filtering effect is not obvious, and the filtering device cannot be widely applied to market demands. Chinese patent CN204310984U discloses a seven-tower multi-effect differential pressure distillation apparatus for co-producing superior alcohol and fuel ethanol, which can co-produce superior alcohol and fuel ethanol, but cannot produce electronic grade anhydrous ethanol at the same time.
SUMMERY OF THE UTILITY MODEL
In view of this, the utility model discloses it is expected to provide a device of production fuel ethanol, electron level ethanol, the utility model discloses can produce two kinds of products of fuel ethanol and electron level absolute ethyl alcohol simultaneously in one set of device, adopt rectification-steam infiltration coupling mode simultaneously, effectively utilize the abundant heat energy of device, realize the abundant cyclic utilization of energy, reach reduce cost and environment-friendly purpose.
In order to achieve the above purpose, the technical scheme of the utility model is realized like this:
the utility model provides a device of production fuel ethanol, electronic grade ethanol, reboiler, flash tank, II rectifying columns at the bottom of reboiler, flash tank, II rectifying columns, II rectifying column top condensers, II rectifying column tower bottom reboilers, condenser, the condenser of condensing tank, its characterized in that at the bottom of II rectifying column tower including feedstock pump, mash preheater, coarse distillation column tower top condenser, I rectifying column tower top condenser, I rectifying column tower: also comprises a vapor permeable membrane separation device and a deionization membrane device; the raw material pump, the mash preheater, the coarse distillation tower, the overhead condenser of the coarse distillation tower and the bottom reboiler of the coarse distillation tower are sequentially communicated through pipelines; the rectifying tower I, the rectifying tower top condenser I, the rectifying tower bottom reboiler I and the flash tank are sequentially communicated through pipelines; the rectifying tower II, a tower top condenser of the rectifying tower II and a reboiler at the tower bottom of the rectifying tower II are sequentially communicated through pipelines; the steam permeable membrane separation device, the condensing tank and the deionization membrane device are sequentially communicated through pipelines; the discharge hole of the mash preheater is connected with a feed inlet pipeline of the coarse distillation tower; the discharge port of the condenser at the top of the rough distillation tower is connected with the feed port pipeline of the rectifying tower I; the discharge hole of the flash tank is connected with the feed inlet pipeline of the rectifying tower II; the discharge port of the condenser at the top of the rectifying tower II is connected with the feed port pipeline of the vapor permeable membrane separation device; a fuel ethanol outlet is formed in a lower pipeline of the condensation tank; the deionization membrane device is provided with an electronic grade ethanol outlet.
Further, the deionization membrane device comprises an ion exchange membrane or a nanofiltration membrane.
Further, the vapor permeable membrane configuration of the vapor permeable membrane separation device comprises a plate type, a tubular type and a hollow fiber type.
Furthermore, the vapor permeable membrane is an organic or inorganic membrane, and comprises a PVA membrane, a NaA molecular sieve membrane, a T-type molecular sieve membrane, an MOR molecular sieve membrane and a ZSM-5 molecular sieve membrane.
The utility model also provides a new technology of production fuel ethanol, electron level ethanol utilizes the above-mentioned device of production fuel ethanol, electron level ethanol, the technology includes following step:
preheating mature mash from a fermentation working section, then feeding the preheated mature mash into the coarse distillation tower, feeding coarse wine with the concentration of 40-60% (v/v) obtained at the top of the coarse distillation tower into the rectifying tower I, and removing water and fusel oil;
high-concentration alcohol with the concentration of 85-95% (v/v) is obtained at the top of the rectifying tower I and enters the rectifying tower II from the flash tank;
meanwhile, about half of mash in the coarse distillation tower is extracted from the coarse distillation tower and enters a rectifying tower II, and after the rectifying tower II is further dehydrated, alcohol steam with the concentration of 85-97% (v/v) is obtained at the tower top;
the alcohol steam enters the steam permeable membrane separation device for deep dehydration, high-purity alcohol steam with the concentration of 99.5-99.9% (v/v) is obtained by membrane residue measurement, feed liquid with the alcohol content of 1-5% (v/v) at the permeation side is conveyed to a mash pool for continuous circulation and recovery, and dehydrated alcohol steam is condensed to obtain a fuel alcohol product;
part of high-purity fuel ethanol products are subjected to ion removal membrane to remove trace ions, and then electronic grade ethanol products are obtained.
Further, mature mash entering the rough distillation tower is preheated by tower kettle waste mash of the rough distillation tower, tower bottom waste liquid of the rectifying tower I and the rectifying tower II and finished absolute ethyl alcohol of the vapor permeable membrane separation device.
Furthermore, the heat of the reboiler at the bottom of the coarse distillation tower is derived from the reflux steam at the top of the rectifying tower II, and the heat of the reboiler at the bottom of the rectifying tower II is derived from the reflux steam at the top of the rectifying tower I.
Further, the operation pressure of the top of the crude distillation tower is 0-0.12 MPa (gauge pressure); the operation temperature of the top of the crude distillation tower is 75-85 ℃; the operation temperature of the bottom of the crude distillation tower is 85-95 ℃.
Further, the operating pressure of the top of the rectifying tower I is 0.2-0.35 MPa (gauge pressure), the temperature of the top of the rectifying tower I is 108-120 ℃, and the temperature of the bottom of the rectifying tower I is 130-150 ℃.
Further, the operating pressure of the top of the rectifying tower II is 0.12-0.2 MPa (gauge pressure); the operating temperature of the top of the rectifying tower II is 95-105 ℃; and the operating temperature of the bottom of the rectifying tower II is 105-115 ℃.
The utility model discloses beneficial effect as follows:
1) the utility model provides a device for producing fuel ethanol and electronic grade ethanol, which can simultaneously produce two products of fuel ethanol and electronic grade ethanol in a set of process device through the coupling of rectification-membrane separation technology, thereby realizing the flexible adjustment of product productivity between the fuel ethanol and the electronic grade ethanol and adapting to the diversified demands of the market;
2) by using the rectification-membrane separation coupling energy-saving process, the surplus heat energy of the device can be effectively utilized, the energy is fully matched and utilized, the steam consumption is saved, the steam unit consumption of the whole system is 1.1-1.4 tons of steam/ton of fuel ethanol product, and the purpose of saving the energy of the system is achieved, and compared with the traditional process, the steam can be saved by more than 20 percent;
3) the whole process flow has the advantages of energy conservation, high efficiency, small occupied area, zero pollution, simple operation, high resource utilization rate and the like, and has huge market application prospect.
Drawings
FIG. 1 is a flow chart of an apparatus for producing fuel ethanol and electronic grade ethanol according to an embodiment of the present invention
Wherein: 1 is a raw material pump; 2 is a mash preheater; 3 is a crude distillation column; 4 is a condensing tank at the top of the crude distillation tower; 5 is a reboiler at the bottom of the crude distillation tower; 6 is a rectifying tower I; 7 is a rectifying tower top condenser I; 8 is a reboiler at the bottom of the rectifying tower I; 9 is a flash tank; 10 is II rectifying tower; 11 is a tower top condenser of the rectifying tower II; 12 is a reboiler at the bottom of the rectifying tower II; 13 is a vapor permeable membrane separation device; 14 is a condensing tank; and 15 is a deionizing membrane unit.
Detailed Description
In order to understand the features and technical contents of the present invention in more detail, the following description is given in conjunction with the accompanying drawings and embodiments, which are only for reference and not for limitation.
The utility model discloses embodiment's core lies in providing a device of production fuel alcohol, electronic grade ethanol, including feedstock pump 1, mash preheater 2, coarse distillation column 3, coarse distillation column top of the tower condenser 4, coarse distillation column reboiler 5 at the bottom of the tower, I rectifying column 6, I rectifying column top of the tower condenser 7, I rectifying column reboiler 8 at the bottom of the tower, flash tank 9, II rectifying column 10, II rectifying column top of the tower condenser 11, II rectifying column reboiler 12 at the bottom of the tower, condensate tank 14, its characterized in that: also comprises a vapor permeable membrane separation device 13 and a deionization membrane device 15; the raw material pump 1, the mash preheater 2, the coarse distillation tower 3, the overhead condenser 4 of the coarse distillation tower and the bottom reboiler 5 of the coarse distillation tower are communicated in sequence through pipelines; the rectifying tower I6, the rectifying tower top condenser 7, the rectifying tower bottom reboiler 8 and the flash tank 9 are communicated in sequence through pipelines; the rectifying tower II 10, the rectifying tower top condenser 11 and the rectifying tower bottom reboiler 12 are communicated in sequence through pipelines; the steam permeable membrane separation device 13, the condensing tank 14 and the deionization membrane device 15 are sequentially communicated through pipelines; the discharge hole of the mash preheater 2 is connected with the feed inlet pipeline of the coarse distillation tower 3; a discharge hole of the condenser 4 at the top of the rough distillation tower is connected with a feed hole pipeline of the rectifying tower 6; the discharge hole of the flash tank 9 is connected with the feed hole pipeline of the rectifying tower 10 of the II; a discharge hole of the condenser 11 at the top of the rectifying tower II is connected with a feed hole pipeline of the vapor permeable membrane separation device 13; a fuel ethanol outlet is arranged on a lower pipeline of the condensation tank 14; the deionization membrane device 15 has an electronic grade ethanol outlet.
Here, the deionization membrane unit 15 includes an ion exchange membrane or a nanofiltration membrane.
Specifically, the operating pressure of the nanofiltration membrane is 0.1-1 MPa (gauge pressure).
Specifically, the pore diameter of the nanofiltration membrane is 5 nm.
Here, the vapor permeable membrane configuration of the vapor permeable membrane separation device 13 includes a plate type, a tube type, and a hollow fiber type.
Preferably, the vapor permeable membrane is an organic or inorganic membrane, and comprises a PVA membrane, a NaA molecular sieve membrane, a T-type molecular sieve membrane, an MOR molecular sieve membrane and a ZSM-5 molecular sieve membrane.
Specifically, the plate, tube, hollow fiber vapor permeable membrane configurations may be composed in one or both of series and parallel connections.
More specifically, the vapor permeable membrane separation device 13 is formed by connecting a plurality of tubular NaA molecular sieve membrane modules in series.
More specifically, the vapor permeable membrane separation device 13 is formed by connecting a plurality of NaA type hollow fiber molecular sieve membrane modules in series.
More specifically, the vapor permeable membrane separation device 13 is formed by combining and connecting a plurality of NaA molecular sieve membranes and T-type molecular sieve membrane modules in series.
The utility model discloses specific embodiment still provides a new technology of apparatus for producing fuel ethanol, electronic grade ethanol, a serial communication port, the technology includes following step:
preheating mature mash from a fermentation working section, then feeding the preheated mature mash into the coarse distillation tower 3, feeding coarse wine with the concentration of 40-60% (v/v) obtained at the top of the coarse distillation tower 3 into the rectifying tower I6, and removing water and fusel oil;
high-concentration alcohol with the concentration of 85-95% (v/v) is obtained at the top of the rectifying tower I6 and enters the rectifying tower II 10 from the flash tank 9;
meanwhile, about half of mash in the coarse distillation tower 3 is extracted from the coarse distillation tower 3 and enters a rectifying tower II 10, and after the rectifying tower II 10 is further dehydrated, alcohol steam with the concentration of 85-97% (v/v) is obtained at the tower top;
the alcohol steam enters the steam permeable membrane separation device 13 for deep dehydration, high-purity alcohol steam with the concentration of 99.5-99.9% (v/v) is obtained by membrane residue measurement, feed liquid with the alcohol content of 1-5% (v/v) at the permeation side is conveyed to a mash pool for continuous circulation and recovery, and the dehydrated alcohol steam is condensed to obtain a fuel alcohol product;
part of high-purity fuel ethanol products are subjected to ion removal membrane to remove trace ions, and then electronic grade ethanol products are obtained.
Here, the mash preheating temperature is 75-80 ℃.
The heat is recycled by adopting differential pressure coupling circulation heat supply, and simultaneously the waste water at the bottom of the rectifying tower and the ethanol steam obtained by membrane dehydration are recycled before being discharged out of the system.
Specifically, the mature mash entering the coarse distillation tower 3 is preheated by tower bottom waste mash of the coarse distillation tower 3, tower bottom waste liquid of the rectifying tower I6, tower bottom waste liquid of the rectifying tower II 10 and finished anhydrous ethanol of the vapor permeation membrane separation device 13.
Here, the heat of the reboiler 5 at the bottom of the crude distillation tower is derived from the reflux steam at the top of the rectifying tower 10 of II, and the heat of the reboiler 12 at the bottom of the rectifying tower of II is derived from the reflux steam at the top of the rectifying tower 6 of I.
Here, the dehydration process can overcome the limitation of gas-liquid equilibrium without introducing a third component, and simultaneously can avoid the defect of complicated process flow of the traditional process.
The relative volatility of the ethanol and the water is high, so that the separation efficiency of the ethanol and the water in the rectifying tower is improved; the steam output from the top of the rectifying tower directly enters the steam permeable membrane separation device 13, and no additional steam heat supply is needed, so that the dehydration rate of the steam permeable membrane separation device 13 is increased, a high-purity product is obtained, and the energy consumption is obviously saved.
Here, the ethanol feed liquid entering the vapor permeable membrane separation device 13 is the alcohol vapor at the top of the II fine tower 10.
Here, the top vapor of the rectifying column II 10 serves as the heating medium for the rectifying column II 3, and the top vapor of the rectifying column I6 serves as the heating medium for the rectifying column II 10.
Here, the operation pressure at the top of the crude distillation column 3 is 0 to 0.12MPa (gauge pressure); the operation temperature of the top of the coarse distillation tower 3 is 75-85 ℃; the operation temperature of the bottom of the crude distillation tower 3 is 85-95 ℃.
Here, the operating pressure at the top of the rectifying column I6 is 0.2 to 0.35MPa (gauge pressure), the temperature at the top of the rectifying column I6 is 108 to 120 ℃, and the temperature at the bottom of the rectifying column I6 is 130 to 150 ℃.
Here, the operating pressure at the top of the rectifying column II 10 is 0.12 to 0.2MPa (gauge pressure); the operating temperature of the top of the rectifying tower 10 of the rectifying tower II is 95-105 ℃; the operation temperature of the tower bottom of the II rectifying tower 10 is 105-115 ℃.
The single anion of the electronic grade absolute ethyl alcohol after the ion removal of the deionization membrane device is controlled below 1ppm, and the cation is controlled below 10 ppb.
Here, the high purity fuel ethanol product has a water content of < 0.1%.
Example 1:
mature mash (the volume content of ethanol is 10%) from a fermentation working section is preheated to 75 ℃ by a mash preheater 2 together with waste mash of a rough distillation tower 3 and finished anhydrous alcohol, and enters the rough distillation tower 3, and waste mash discharged from a tower kettle of the rough distillation tower 3 exchanges heat with the mature mash and enters a wastewater treatment system. The operation pressure at the top of the crude distillation tower 3 is controlled to be 0.1MPa, the temperature at the top of the tower is controlled to be 78 ℃, and the temperature at the bottom of the tower is controlled to be 85 ℃. To obtain crude liquor gas with the concentration of 55 percent at the tower top.
The crude wine steam with the concentration of 55 percent at the top of the crude distillation tower 3 is used as the feed of the rectifying tower I6, and the water and the fusel oil are removed by the rectifying tower I6. Heating by a reboiler 8 at the bottom of the rectifying tower I to control the temperature at the bottom of the rectifying tower to be 135 ℃; i, the operating pressure of a rectifying tower 6 is 0.25 Mpa; the operation temperature at the top of the rectifying tower is 110 ℃, and high-concentration ethanol with the concentration of 90% (v/v) is obtained at the top of the rectifying tower I.
The high-concentration ethanol obtained by the rectifying tower I6 enters a rectifying tower II 10 from a flash tank 9, meanwhile, about half of mash in the coarse distillation tower 3 is extracted from the coarse distillation tower 3 and enters the rectifying tower II 10, tower top steam of the rectifying tower I6 is used as a heating medium of the rectifying tower II 10 for heating, the tower bottom operating temperature of the rectifying tower II 10 is controlled to be 105 ℃, the operating pressure is kept to be 0.15Mpa, and the tower top operating temperature is 98 ℃; the high-purity ethanol steam with the concentration of 90% (v/v) is obtained at the top of the tower.
And the high-purity ethanol steam extracted from the rectifying tower II 10 enters a steam permeable membrane separation device 13 for deep dehydration. Wherein, the vapor permeable membrane separation device 13 is formed by connecting a plurality of tubular NaA molecular sieve membrane components in series, and the total filtration area reaches 280m2The permeable side of the vapor permeable membrane is pumped by a vacuum pump, the vacuum degree is 1000pa, ethanol and water are subjected to vapor permeation separation on a molecular sieve membrane, the ethanol content of the permeated liquid is pumped out from the permeable side of the vapor permeable membrane and is about 1% (v/v), and the permeated liquid is collected after being cooled and conveyed to a mash pool by a pump. High-purity ethanol steam with the concentration of 99.9 percent is obtained by a pervaporation membrane separation device, and the dehydrated ethanol steam is condensed by a condensing tank 14 to obtain a fuel ethanol product.
99.9 percent of absolute ethyl alcohol separated by the vapor permeable membrane separation device 13 passes through a deionization membrane device 15, wherein the deionization membrane device 15 is an anion-cation exchange membrane, and the ultra-pure electronic grade absolute ethyl alcohol is obtained after filtration.
Example 2:
mature mash (ethanol volume content is 5%) from a fermentation working section is preheated to 80 ℃ by a mash preheater 2, enters a coarse distillation tower 3 together with waste mash of the coarse distillation tower 3 and finished anhydrous alcohol, and enters a wastewater treatment system after the waste mash discharged from a tower kettle of the coarse distillation tower 3 exchanges heat with the mature mash. The operation pressure at the top of the crude distillation tower 3 is controlled to be 0.12MPa, the temperature at the top of the tower is 85 ℃, and the temperature at the bottom of the tower is 90 ℃. To obtain crude liquor gas with the concentration of 55 percent at the tower top.
The crude wine steam with the concentration of 55 percent at the top of the crude distillation tower 3 is used as the feed of the rectifying tower I6, and the water and the fusel oil are removed by the rectifying tower I6. Heating by a reboiler 8 at the bottom of the rectifying tower I to control the temperature at the bottom of the rectifying tower to be 140 ℃; i, the operating pressure of a rectifying tower 6 is 0.3 Mpa; the operation temperature of the top of the rectifying tower is 118 ℃, and high-concentration ethanol with the concentration of 90% (v/v) is obtained at the top of the rectifying tower I.
The high-concentration ethanol obtained by the rectifying tower I6 enters a rectifying tower II 10 from a flash tank 9, meanwhile, about half of mash in the coarse distillation tower 3 is extracted from the coarse distillation tower 3 and enters the rectifying tower II 10, tower top steam of the rectifying tower I6 is used as a heating medium of the rectifying tower II 10 for heating, the tower bottom operating temperature of the rectifying tower II 10 is controlled to be 110 ℃, the operating pressure is kept to be 0.2Mpa, and the tower top operating temperature is 100 ℃; the high-purity ethanol steam with the concentration of 93 percent (v/v) is obtained at the top of the tower.
And the high-purity ethanol steam extracted from the rectifying tower II 10 enters a steam permeable membrane separation device 13 for deep dehydration. Wherein, the vapor permeable membrane separation device 13 is formed by connecting a plurality of NaA type hollow fiber molecular sieve membrane components in series, and the total filling area is 160m2The permeable side of the vapor permeable membrane is pumped by a vacuum pump, the vacuum degree is 1000pa, ethanol and water are subjected to vapor permeation separation on a molecular sieve membrane, the ethanol content of the permeated liquid is pumped out from the permeable side of the vapor permeable membrane and is about 1% (v/v), and the permeated liquid is collected after being cooled and conveyed to a mash pool by a pump. High-purity ethanol steam with the concentration of 99.9 percent is obtained by a pervaporation membrane separation device, and the dehydrated ethanol steam is condensed by a condensing tank 14 to obtain a fuel ethanol product.
99.9 percent of absolute ethyl alcohol separated by the vapor permeable membrane separation device 13 passes through a deionization membrane device 15, wherein the deionization membrane device 15 is a nanofiltration membrane, the membrane aperture is 5nm, the nanofiltration membrane filtering operation pressure is 0.3Mpa, and the ultra-pure electronic grade absolute ethyl alcohol is obtained after filtering.
Example 3:
mature mash (the volume content of ethanol is 13%) from a fermentation working section is preheated to 80 ℃ by a mash preheater 2, enters a coarse distillation tower 3 together with waste mash of the coarse distillation tower 3 and finished anhydrous alcohol, and enters a wastewater treatment system after the waste mash discharged from a tower kettle of the coarse distillation tower 3 exchanges heat with the mature mash. The operation pressure at the top of the crude distillation tower 3 is controlled to be 0.12MPa, the temperature at the top of the tower is 85 ℃, and the temperature at the bottom of the tower is 90 ℃. To obtain crude liquor gas with the concentration of 55 percent at the tower top.
The crude wine steam with the concentration of 55 percent at the top of the crude distillation tower 3 is used as the feed of the rectifying tower I6, and the water and the fusel oil are removed by the rectifying tower I6. Heating by a reboiler 8 at the bottom of the rectifying tower I to control the temperature at the bottom of the rectifying tower to be 145 ℃; i, the operating pressure of a rectifying tower 6 is 0.3 Mpa; the operation temperature at the top of the rectifying tower is 120 ℃, and high-concentration ethanol with the concentration of 90% (v/v) is obtained at the top of the rectifying tower I.
The high-concentration ethanol obtained by the rectifying tower I6 enters a rectifying tower II 10 from a flash tank 9, meanwhile, about half of mash in the coarse distillation tower 3 is extracted from the coarse distillation tower 3 and enters the rectifying tower II 10, tower top steam of the rectifying tower I6 is used as a heating medium of the rectifying tower II 10 for heating, the tower bottom operating temperature of the rectifying tower II 10 is controlled to be 110 ℃, the operating pressure is kept to be 0.2Mpa, and the tower top operating temperature is 100 ℃; the high-purity ethanol steam with the concentration of 95.5% (v/v) is obtained at the top of the tower.
And the high-purity ethanol steam extracted from the rectifying tower II 10 enters a steam permeable membrane separation device 13 for deep dehydration. Wherein, the vapor permeable membrane separation device 13 is formed by combining and connecting a plurality of NaA molecular sieve membranes and T-shaped molecular sieve membrane components in series, and the total filling area is 260m2The permeable side of the vapor permeable membrane is pumped by a vacuum pump, the vacuum degree is 1000pa, ethanol and water are subjected to vapor permeation separation on a molecular sieve membrane, the ethanol content of the permeated liquid is pumped out from the permeable side of the vapor permeable membrane and is about 1% (v/v), and the permeated liquid is collected after being cooled and conveyed to a mash pool by a pump. High-purity ethanol steam with the concentration of 99.9 percent is obtained by a pervaporation membrane separation device, and the dehydrated ethanol steam is condensed by a condensing tank 14 to obtain a fuel ethanol product.
99.9 percent of absolute ethyl alcohol separated by the vapor permeable membrane separation device 13 passes through a deionization membrane device 15, wherein the deionization membrane device 15 is a nanofiltration membrane, the membrane aperture is 5nm, the nanofiltration membrane filtering operation pressure is 0.3Mpa, and the ultra-pure electronic grade absolute ethyl alcohol is obtained after filtering.
The above-mentioned general knowledge is not described in detail, and can be understood by those skilled in the art.
The above description is only exemplary of the present invention and should not be construed as limiting the present invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. The utility model provides a device of production fuel ethanol, electronic grade ethanol, including feedstock pump (1), mash preheater (2), gas retort (3), gas retort overhead condenser (4), gas retort reboiler (5) at the bottom of the gas retort tower, I rectifying column (6), I rectifying column overhead condenser (7), reboiler (8) at the bottom of I rectifying column tower, flash tank (9), II rectifying column (10), II rectifying column overhead condenser (11), reboiler (12) at the bottom of II rectifying column tower, condensing tank (14), its characterized in that: also comprises a vapor permeable membrane separation device (13) and a deionization membrane device (15); the raw material pump (1), the mash preheater (2), the coarse distillation tower (3), the overhead condenser (4) of the coarse distillation tower and the bottom reboiler (5) of the coarse distillation tower are sequentially communicated through pipelines; the rectifying tower I (6), the rectifying tower top condenser I (7), the rectifying tower bottom reboiler I (8) and the flash tank I (9) are communicated in sequence through pipelines; the rectifying tower II (10), a rectifying tower top condenser (11) and a rectifying tower bottom reboiler (12) are communicated in sequence through pipelines; the vapor permeable membrane separation device (13), the condensing tank (14) and the deionization membrane device (15) are communicated in sequence through pipelines; the discharge hole of the mash preheater (2) is connected with the feed inlet pipeline of the coarse distillation tower (3); the discharge hole of the condenser (4) at the top of the rough distillation tower is connected with the feed hole of the rectifying tower (6) through a pipeline; the discharge hole of the flash tank (9) is connected with the feed hole of the rectifying tower (10) II through a pipeline; the discharge hole of the condenser (11) at the top of the rectifying tower II is connected with the feed hole pipeline of the vapor permeable membrane separation device (13); a fuel ethanol outlet is arranged on a lower pipeline of the condensation tank (14); the deionization membrane device (15) is provided with an electronic grade ethanol outlet.
2. The apparatus for producing fuel ethanol, electronic grade ethanol, according to claim 1, wherein: the deionization membrane device (15) comprises an ion exchange membrane or a nanofiltration membrane.
3. The apparatus for producing fuel ethanol, electronic grade ethanol, according to claim 2, wherein: the operating pressure of the nanofiltration membrane is 0.1-1 MPa.
4. The apparatus for producing fuel ethanol, electronic grade ethanol, according to claim 2, wherein: the aperture of the nanofiltration membrane is 5 nm.
5. The apparatus for producing fuel ethanol, electronic grade ethanol, according to claim 1, wherein: the steam permeable membrane configuration of the steam permeable membrane separation device (13) comprises a plate type, a tubular type and a hollow fiber type.
6. The apparatus for producing fuel ethanol, electronic grade ethanol, according to claim 5, wherein: the vapor permeable membrane is an organic or inorganic membrane and comprises a PVA membrane, a NaA molecular sieve membrane, a T-shaped molecular sieve membrane, an MOR molecular sieve membrane and a ZSM-5 molecular sieve membrane.
7. The apparatus for producing fuel ethanol, electronic grade ethanol, according to claim 6, wherein: the plate type, tubular type and hollow fiber type vapor permeable membrane configuration is formed in one or two modes of series connection and parallel connection.
8. The apparatus for producing fuel ethanol, electronic grade ethanol, according to claim 7, wherein: the vapor permeable membrane separation device (13) is formed by connecting a plurality of tubular NaA molecular sieve membrane components in series.
9. The apparatus for producing fuel ethanol, electronic grade ethanol, according to claim 7, wherein: the vapor permeable membrane separation device (13) is formed by connecting a plurality of NaA type hollow fiber molecular sieve membrane components in series.
10. The apparatus for producing fuel ethanol, electronic grade ethanol, according to claim 7, wherein: the vapor permeable membrane separation device (13) is formed by combining and connecting a plurality of NaA molecular sieve membranes and T-shaped molecular sieve membrane assemblies in series.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201922009606.2U CN211078979U (en) | 2019-11-20 | 2019-11-20 | Device for producing fuel ethanol and electronic grade ethanol |
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| CN201922009606.2U CN211078979U (en) | 2019-11-20 | 2019-11-20 | Device for producing fuel ethanol and electronic grade ethanol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114712884A (en) * | 2022-06-08 | 2022-07-08 | 北京化工大学 | Device and method for producing electronic grade ethanol by rectification-membrane separation |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114712884A (en) * | 2022-06-08 | 2022-07-08 | 北京化工大学 | Device and method for producing electronic grade ethanol by rectification-membrane separation |
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