CN107162875A - A kind of technique and system that refined methanol and absolute ethyl alcohol are extracted from crude carbinol - Google Patents
A kind of technique and system that refined methanol and absolute ethyl alcohol are extracted from crude carbinol Download PDFInfo
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- CN107162875A CN107162875A CN201710488446.7A CN201710488446A CN107162875A CN 107162875 A CN107162875 A CN 107162875A CN 201710488446 A CN201710488446 A CN 201710488446A CN 107162875 A CN107162875 A CN 107162875A
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- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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Abstract
The present invention relates to a kind of technique and system that refined methanol and absolute ethyl alcohol are extracted from crude carbinol, processing step is：After crude carbinol is handled through pre-rectifying tower, periodic off-gases scrubbing tower, compression rectification tower, atmospheric distillation tower, recovery tower, fusel oil rectifier, membrane filtration dewatering system, methanol distillation column, Ethanol rectification column etc., the products such as refined methanol, absolute ethyl alcohol, anhydrous C4 fusels, fusel oil are can obtain.The present invention is using crude carbinol as raw material, carry out the technical process such as systematically rectifying and membrane filtration dehydration, with energy-conservation, it is efficient the characteristics of, the products such as the present invention can as needed separate and obtain methanol, absolute ethyl alcohol, anhydrous C4 fusels, fusel oil, wherein fusel oil and anhydrous C4 fusels can be used as gasoline blend component, the present invention can improve the added value of ammonia from coal device to greatest extent, with significant economic benefit and social benefit.
Description
Technical field
The present invention relates to a kind of technique and system that refined methanol and absolute ethyl alcohol are extracted from crude carbinol, belong to ammonia from coal
Technical field.
Background technology
It is general that refined methanol is obtained using the rectification process of crude carbinol in ammonia from coal technique.Traditional crude carbinol rectifying
Technique typically uses three towers or four-column process flow, in addition to refined methanol is obtained, and also obtains water content very high rectifying accessory substance, simultaneously
The accessory substance contains a certain amount of methanol.Water content very high rectifying accessory substance poor quality, it is impossible to directly apply, if directly row
Put and will result in environmental pollution, cost of sewage disposal, and content of organics high disposal can be increased again by being discharged to sewage disposal process
It is also difficult for getting up.
The content of the invention
The invention provides a kind of technique and system that refined methanol and absolute ethyl alcohol are extracted from crude carbinol, the present invention is used
Rectifying and the technique of UF membrane coupling, extract refined methanol, absolute ethyl alcohol, fusel oil, anhydrous C4 fusels etc. a variety of from crude carbinol
Product, fusel oil and anhydrous C4 fusels can as gasoline blend component, fusel oil can be made to get utilization, subtracted
Few environmental pollution, invention significantly improves the economic benefit of ammonia from coal device and social benefit, solves traditional rectifying work
The higher rectifying accessory substance of water content that skill is obtained can not recycling problem.Technical scheme is as follows：
A kind of technique that refined methanol and absolute ethyl alcohol are extracted from crude carbinol, is comprised the following steps that：
（1）Crude carbinol enters pre-rectifying tower, after the overhead components of pre-rectifying tower exchange heat through heat exchanger B, gas after being exchanged heat through heat exchanger A
Mutually part enters periodic off-gases scrubbing tower, and gas phase portion contains substantial amounts of methanol, is reclaimed into periodic off-gases scrubbing tower in gas phase portion
Methanol, liquid phase part enter backflash A, the separation of aqueous phase and fusel oil, the tower of periodic off-gases scrubbing tower are realized in backflash A
Enter pre-rectifying tower, backflash A top light component after pushing up the bottom component mixing for fuel gas, bottom of towe component and backflash A
For fusel oil, can individually it reclaim；
The pre-rectifying tower tower top pressure is 139 kPaA, and temperature is 74.8 DEG C；Tower bottom pressure is that 147 kPaA temperature are 77.5
DEG C, reflux ratio is 0.92；The temperature of the pressure normal pressure of periodic off-gases scrubbing tower, tower top and bottom of towe is in normal temperature, periodic off-gases scrubbing tower
Provided with desalination water spray system, positioned at gas phase entrance top, desalted water and gaseous component counter current contacting are to wash the first in gas phase
Alcohol.
（2）The bottom of towe component of pre-rectifying tower enters compression rectification tower, pre-rectifying tower and compression rectification after being exchanged heat through heat exchanger C
Tower shares a heat exchanger C；
The tower top pressure of the compression rectification tower is 800 kPaA, and temperature is 128 DEG C；Tower bottom pressure is 813 kPaA, and temperature is
134℃；Reflux ratio is 3.0.
（3）The overhead components of compression rectification tower are divided into two parts after backflash B, and a part exchanges heat laggard through heat exchanger D
Enter compression rectification tower as backflow, another part as industrial methanol finished product, the bottom component of compression rectification tower is changed through heat exchanger C
Enter atmospheric distillation tower after heat；
The purpose of overhead reflux allows the more solutes absorbed in fogs of liquid flux for more preferable stripping, reaches more preferable vapour
Liquid rectification effect；Another part is extracted out and is used as industrial methanol finished product.
（4）The overhead components of atmospheric distillation tower enter backflash C, the component come out from backflash C after being exchanged heat through heat exchanger E
Be divided into three strands, one enter atmospheric distillation tower as overhead reflux, a stock-traders' know-how heat exchanger F heat exchange after as industrial methanol finished product,
One enters recovery tower as overhead reflux, and the bottom of towe component of atmospheric distillation tower is discharged into waste water after being exchanged heat for waste water through heat exchanger G
System；
The tower top pressure of the atmospheric distillation tower is 113 kPaA, and temperature is 67.5 DEG C；Tower bottom pressure is 143 kPaA, and temperature is
110℃；Reflux ratio is 1.85.
（5）The component come out from atmospheric distillation tower enters recovery tower lower end through feeder trough, and the overhead components of recovery tower enter normal pressure
Rectifying column, bottom of towe component are to be discharged into waste water system after waste water exchanges heat through heat exchanger H, and the lower end component of recovery tower is changed through heat exchanger I
Enter fusel oil rectifying column after heat；
The tower top pressure of the recovery tower is 133 kPaA, and temperature is 72 DEG C；Tower bottom pressure is 153 kPaA, and temperature is 111.5
℃；Capacity of returns 3100kg/h.
（6）The overhead components of fusel oil rectifier enter backflash D after being exchanged heat through heat exchanger J, go out backflash D component point
For two strands, one return again to fusel oil rectifier as overhead reflux, another stock it is aqueous be less than 10% fusel it is de- into membrane filtration
Water system, the bottom of towe component of fusel oil rectifier enters waste water system after being exchanged heat through heat exchanger K, tower lower end another part is through heat exchange
Fusel oil rectifier is returned after device L heat exchange；
The tower top pressure of the fusel oil rectifier is 23 kPaA, and temperature is 99.45 DEG C；Tower bottom pressure is 30 kPaA, temperature
For 100 DEG C；Reflux ratio is 12-13；It is preferred that, reflux ratio is 12.5.
（7）Most of waste water in membrane filtration dewatering system removing fusel, aqueous 0.5% fusel of being no more than is returned into methanol
Receive tower；
（8）The overhead components of methanol distillation column are divided into two strands after heat exchanger M and backflash E, and one makees into methanol distillation column
For overhead reflux, the overhead product of another stock and recovery tower enters atmospheric distillation tower, the bottom of towe component one of methanol distillation column together
Part returns to methanol distillation column after being exchanged heat through heat exchanger N and flowed back as bottom of towe, is partly into Ethanol rectification column as ethanol essence
Evaporate the charging of tower；
The pressure of the methanol distillation column is normal pressure, and tower top temperature is 69 DEG C, and column bottom temperature is 79 DEG C.
（9）The overhead components of Ethanol rectification column enter backflash F after being exchanged heat through heat exchanger O, and the component for going out backflash F is divided into
Two strands, one enters Ethanol rectification column as overhead reflux, and the absolute ethyl alcohol of high-purity is obtained after stock-traders' know-how heat exchanger P heat exchange,
A bottom of towe component part for Ethanol rectification column returns to Ethanol rectification column after being exchanged heat through heat exchanger Q and flowed back as bottom of towe, another part
Anhydrous C4 fusels are obtained after being exchanged heat through heat exchanger R；
The pressure of the Ethanol rectification column is normal pressure, and tower top temperature is 78.5 DEG C, and column bottom temperature is 83 DEG C.
Heretofore described pre-rectifying tower, compression rectification tower, atmospheric distillation tower, recovery tower, fusel oil rectifier, methanol are returned
The combination tower of column plate can be added using plate column or structured packing by receiving tower and Ethanol rectification column, and preferably structured packing adds column plate
Combination tower.
In the present invention, the system that refined methanol and absolute ethyl alcohol are extracted from crude carbinol, system includes periodic off-gases scrubbing tower, pre-
Rectifying column, compression rectification tower, atmospheric distillation tower, recovery tower, fusel oil rectifier, membrane filtration dewatering system, methanol distillation column and
Ethanol rectification column；Heat exchanger A is connected by pipeline with pre-rectifying tower, and the tower top of pre-rectifying tower is connected by pipeline with heat exchanger B,
Heat exchanger B is connected with periodic off-gases scrubbing tower and backflash A respectively by pipeline, the bottom of towe of periodic off-gases scrubbing tower and backflash A's
Bottom is connected by pipeline with pre-rectifying tower, and pre-rectifying tower bottom of towe is connected by pipeline through heat exchanger C with compression rectification tower, pressurization
Rectifying tower bottom is connected by pipeline through heat exchanger C with atmospheric distillation tower, and compression rectification column overhead is connected by pipeline and backflash B
Connect, backflash B is connected with industrial methanol accumulator tank and heat exchanger D respectively by pipeline, and heat exchanger D passes through pipeline and compression rectification
Tower is connected, and atmospheric distillation column overhead is connected by pipeline with heat exchanger E, and heat exchanger E is connected by pipeline with backflash C, backflow
Groove C is connected with atmospheric distillation tower, recovery tower and heat exchanger F respectively by pipeline, and heat exchanger F is stored by pipeline and industrial methanol
Groove is connected, and atmospheric distillation tower bottom of towe is connected by pipeline with heat exchanger G, and atmospheric distillation tower is by pipeline through feeder trough and recovery tower
It is connected, reclaims column overhead and be connected by pipeline with atmospheric distillation tower, recovery tower bottom of towe is connected by pipeline with heat exchanger H, reclaim
Tower is connected by pipeline through heat exchanger I with fusel oil rectifier, and the bottom of towe of fusel oil rectifier passes through pipeline and heat exchanger K phases
Even, fusel oil rectifier lower end is connected by pipeline with heat exchanger L, and heat exchanger L is connected by pipeline with fusel oil rectifier, miscellaneous
Alcohol oil rectifier tower top is connected by pipeline through heat exchanger J with backflash D, backflash D by pipeline respectively with fusel oil rectifying
Tower is connected with membrane filtration dewatering system, and membrane filtration dewatering system is connected by pipeline with methanol distillation column, and Methanol Recovery tower top leads to
Piping is connected through heat exchanger M with backflash E, and backflash E is connected with methanol distillation column and atmospheric distillation tower respectively by pipeline,
Methanol distillation column bottom of towe is connected with heat exchanger N and Ethanol rectification column respectively by pipeline, and heat exchanger N passes through pipeline and Methanol Recovery
Tower be connected, Ethanol rectification column tower top is connected by pipeline through heat exchanger O with backflash F, backflash F by pipeline respectively with ethanol
Rectifying column is connected with heat exchanger P, and heat exchanger P is connected by pipeline with absolute ethyl alcohol accumulator tank, and Ethanol rectification column bottom of towe passes through pipe
Road is connected with heat exchanger Q and heat exchanger R respectively, and heat exchanger Q is connected by pipeline with Ethanol rectification column, and heat exchanger R passes through pipeline
Be connected with anhydrous C4 fusels accumulator tank, heat exchanger G, heat exchanger H, heat exchanger K and membrane filtration dewatering system bottom and waste water
System is connected.
Further, the membrane filtration dewatering system include feeder trough A, superheater, membrane module, vavuum pump, water storage tank and
Pan tank, the feeder trough A is connected by pipeline through heat exchanger one with superheater, and superheater is connected by pipeline with membrane module,
Membrane module is connected by pipeline through heat exchanger two with water storage tank, and membrane module is connected by pipeline through heat exchanger three with pan tank, water
Storage tank is connected by pipeline with vavuum pump；It is preferred that, mixed between the membrane module using series, parallel or series and parallel
Mode；The vavuum pump is water-ring vacuum pump；The membrane module is inorganic infiltrating and vaporizing membrane.
The present invention has advantages below compared with prior art：
（1）The technique that the present invention is coupled using rectifying and UF membrane, solves traditional rectification process and obtains the higher essence of water content
Evaporate accessory substance can not recycling problem；
（2）The present invention can obtain the multiple products such as refined methanol, absolute ethyl alcohol, fusel oil, anhydrous C4 fusels as needed, and miscellaneous
The oily and anhydrous C4 fusels of alcohol can as gasoline blend component；
（3）The present invention can make fusel oil get utilization, and reduce environmental pollution, while significantly improving ammonia from coal dress
The economic benefit and social benefit put；
（4）The present invention can reclaim the methanol escaped from pre-rectifying tower tower top to greatest extent, and recyclable fusel oil.
Brief description of the drawings
Fig. 1 is present invention process flow chart；
Fig. 2 is membrane filtration dewatering system flow chart.
Symbol description：
1. periodic off-gases scrubbing tower, 2. pre-rectifying towers, 3. compression rectification towers, 4. atmospheric distillation towers, 5. recovery towers, 6. fusel olein
Evaporate tower, 7. membrane filtration dewatering systems, 8. methanol distillation columns, 9. Ethanol rectification columns, 10-27. heat exchanger A-R, 28-33. backflashes
A-F, 34. feeder troughs, 35. industrial methanol accumulator tanks, 36. absolute ethyl alcohol accumulator tanks, 37. anhydrous C4 fusels accumulator tanks, 701. are given
Hopper A, 702. superheaters, 703. membrane modules, 704. vavuum pumps, 705. water storage tanks, 706. pan tanks, 707. heat exchangers one,
708. heat exchangers two, 709. heat exchangers three.
Embodiment
The invention will now be further described with reference to specific embodiments, advantages of the present invention and feature will be with description and
It is apparent.But embodiment is only exemplary, does not constitute any limitation to the scope of the present invention.Those skilled in the art should
It should be appreciated that, the details and form of technical solution of the present invention can be repaiied without departing from the spirit and scope of the invention
Change or replace, but these modifications and replacement are each fallen within protection scope of the present invention.
In the present invention, pre-rectifying tower, compression rectification tower, atmospheric distillation tower, recovery tower, fusel oil rectifier, Methanol Recovery
Tower and Ethanol rectification column are the combination tower of structured packing plus column plate.
A kind of technique that refined methanol and absolute ethyl alcohol are extracted from crude carbinol of embodiment 1
Comprise the following steps that：
（1）Crude carbinol enters pre-rectifying tower 2 after being exchanged heat through heat exchanger A 10, and the overhead components of pre-rectifying tower 2 are through heat exchanger B 11
After heat exchange, gas phase portion enters periodic off-gases scrubbing tower 1, and gas phase portion contains substantial amounts of methanol, reclaimed into periodic off-gases scrubbing tower 1
Methanol in gas phase portion, liquid phase part enters backflash A 28, and the separation of aqueous phase and fusel oil is realized in backflash A 28,
The tower top of periodic off-gases scrubbing tower 1 enters pre-rectifying tower after being mixed for the bottom component of fuel gas, bottom of towe component and backflash A 28
2, backflash A 28 top light component are fusel oil, can individually be reclaimed；
（2）The bottom of towe component of pre-rectifying tower 2 enters compression rectification tower 3, pre-rectifying tower 2 and pressurization essence after being exchanged heat through heat exchanger C 12
Evaporate tower 3 and share a heat exchanger C 12；
（3）The overhead components of compression rectification tower 3 are divided into two parts after backflash B 29, after a part exchanges heat through heat exchanger D 13
Into compression rectification tower 3 as backflow, another part as industrial methanol finished product, the bottom component of compression rectification tower 3 is through heat exchange
Device C 12 enters atmospheric distillation tower 4 after exchanging heat；
（4）The overhead components of atmospheric distillation tower 4 enter backflash C 30 after being exchanged heat through heat exchanger E 14, are come out from backflash C 30
Component be divided into three strands, one enter atmospheric distillation tower 4 as overhead reflux, a stock-traders' know-how heat exchanger F 15 heat exchange after as industry
Methanol finished product, one enter recovery tower 5 as overhead reflux, the bottom of towe component of atmospheric distillation tower 4 is waste water through heat exchanger G 16
Waste water system is discharged into after heat exchange；
（5）Enter the lower end of recovery tower 5 from the component of atmospheric distillation tower 4 out through feeder trough 34, the overhead components of recovery tower 5 enter
Atmospheric distillation tower 4, bottom of towe component are that waste water system is discharged into after waste water exchanges heat through heat exchanger H 17, the lower end component warp of recovery tower 5
Heat exchanger I 18 enters fusel oil rectifying column 6 after exchanging heat；
（6）The overhead components of fusel oil rectifier 6 enter backflash D 31 after being exchanged heat through heat exchanger J 19, go out backflash D's 31
Component is divided into two strands, and one returns again to fusel oil rectifier 6 and entered as aqueous 10% fusel of being less than of overhead reflux, another stock
Membrane filtration dewatering system 7, the bottom of towe component of fusel oil rectifier 6 enters waste water system, tower lower end after being exchanged heat through heat exchanger K 20
Another part returns to fusel oil rectifier 6 after being exchanged heat through heat exchanger L 21；
（7）Most of waste water in the removing fusel of membrane filtration dewatering system 7, aqueous 0.5% fusel of being no more than enters methanol distillation column
8；
（8）The overhead components of methanol distillation column 8 are divided into two strands after heat exchanger M 22 and backflash E 32, and one is returned into methanol
Tower 8 is received as overhead reflux, the overhead product of another stock and recovery tower 5 enters atmospheric distillation tower 4 together, methanol distillation column 8
A bottom of towe component part returns to methanol distillation column 8 after being exchanged heat through heat exchanger N 23 and flowed back as bottom of towe, is partly into ethanol essence
Tower 9 is evaporated as the charging of Ethanol rectification column；
（9）The overhead components of Ethanol rectification column 9 enter backflash F 33 after being exchanged heat through heat exchanger O 24, go out backflash F 33 group
It is divided into two strands, one enters Ethanol rectification column 9 as overhead reflux, and high-purity is obtained after a stock-traders' know-how heat exchanger P 25 heat exchange
Absolute ethyl alcohol, a bottom of towe component part for Ethanol rectification column 9 returns to Ethanol rectification column 9 after being exchanged heat through heat exchanger Q 26 and is used as bottom of towe
Backflow, another part obtains anhydrous C4 fusels after being exchanged heat through heat exchanger R 27.
A kind of technique that refined methanol and absolute ethyl alcohol are extracted from crude carbinol of embodiment 2
Comprise the following steps that：
（1）Crude carbinol enters pre-rectifying tower 2 after being exchanged heat through heat exchanger A 10, and the overhead components of pre-rectifying tower 2 are through heat exchanger B 11
After heat exchange, gas phase portion enters periodic off-gases scrubbing tower 1, and gas phase portion contains substantial amounts of methanol, reclaimed into periodic off-gases scrubbing tower 1
Methanol in gas phase portion, liquid phase part enters backflash A 28, and the separation of aqueous phase and fusel oil is realized in backflash A 28,
The tower top of periodic off-gases scrubbing tower 1 enters pre-rectifying tower after being mixed for the bottom component of fuel gas, bottom of towe component and backflash A 28
2, backflash A 28 top light component are fusel oil, can individually be reclaimed；
The tower top pressure of pre-rectifying tower 2 is 139 kPaA, and temperature is 74.8 DEG C；Tower bottom pressure is that 147 kPaA temperature are 77.5
DEG C, reflux ratio is 0.92；The temperature of the pressure normal pressure of periodic off-gases scrubbing tower 1, tower top and bottom of towe is normal temperature, periodic off-gases scrubbing tower 1
It is interior to be provided with desalination water spray system, positioned at gas phase entrance top；
（2）The bottom of towe component of pre-rectifying tower 2 enters compression rectification tower 3, pre-rectifying tower 2 and pressurization essence after being exchanged heat through heat exchanger C 12
Evaporate tower 3 and share a heat exchanger C 12；
The tower top pressure of the compression rectification tower 3 is 800 kPaA, and temperature is 128 DEG C；Tower bottom pressure is 813 kPaA, and temperature is
134℃；Reflux ratio is 3.0；
（3）The overhead components of compression rectification tower 3 are divided into two parts after backflash B 29, after a part exchanges heat through heat exchanger D 13
Into compression rectification tower 3 as backflow, another part as industrial methanol finished product, the bottom component of compression rectification tower 3 is through heat exchange
Device C 12 enters atmospheric distillation tower 4 after exchanging heat；
（4）The overhead components of atmospheric distillation tower 4 enter backflash C 30 after being exchanged heat through heat exchanger E 14, are come out from backflash C 30
Component be divided into three strands, one enter atmospheric distillation tower 4 as overhead reflux, a stock-traders' know-how heat exchanger F 15 heat exchange after as industry
Methanol finished product, one enter recovery tower 5 as overhead reflux, the bottom of towe component of atmospheric distillation tower 4 is waste water through heat exchanger G 16
Waste water system is discharged into after heat exchange；
The tower top pressure of the atmospheric distillation tower 4 is 113 kPaA, and temperature is 67.5 DEG C；Tower bottom pressure is 143 kPaA, temperature
For 110 DEG C；Reflux ratio is 1.85；
（5）Enter the lower end of recovery tower 5 from the component of atmospheric distillation tower 4 out through feeder trough 34, the overhead components of recovery tower 5 enter
Atmospheric distillation tower 4, bottom of towe component are that waste water system is discharged into after waste water exchanges heat through heat exchanger H 17, the lower end component warp of recovery tower 5
Heat exchanger I 18 enters fusel oil rectifying column 6 after exchanging heat；
The tower top pressure of the recovery tower 5 is 133 kPaA, and temperature is 72 DEG C；Tower bottom pressure is 153 kPaA, and temperature is 111.5
℃；Capacity of returns 3100kg/h；
（6）The overhead components of fusel oil rectifier 6 enter backflash D 31 after being exchanged heat through heat exchanger J 19, go out backflash D's 31
Component is divided into two strands, and one returns again to fusel oil rectifier 6 and entered as aqueous 10% fusel of being less than of overhead reflux, another stock
Membrane filtration dewatering system 7, the bottom of towe component of fusel oil rectifier 6 enters waste water system, tower lower end after being exchanged heat through heat exchanger K 20
Another part returns to fusel oil rectifier 6 after being exchanged heat through heat exchanger L 21；
The tower top pressure of the fusel oil rectifier 6 is 23 kPaA, and temperature is 99.45 DEG C；Tower bottom pressure is 30 kPaA, temperature
For 100 DEG C；Reflux ratio is 12.5；
（7）Most of waste water in the removing fusel of membrane filtration dewatering system 7, aqueous 0.5% fusel of being no more than enters methanol distillation column
8；
（8）The overhead components of methanol distillation column 8 are divided into two strands after heat exchanger M 22 and backflash E 32, and one is returned into methanol
Tower 8 is received as overhead reflux, the overhead product of another stock and recovery tower 5 enters atmospheric distillation tower 4 together, methanol distillation column 8
A bottom of towe component part returns to methanol distillation column 8 after being exchanged heat through heat exchanger N 23 and flowed back as bottom of towe, is partly into ethanol essence
Tower 9 is evaporated as the charging of Ethanol rectification column；
The pressure of the methanol distillation column 8 is normal pressure, and tower top temperature is 69 DEG C, and column bottom temperature is 79 DEG C；
（9）The overhead components of Ethanol rectification column 9 enter backflash F 33 after being exchanged heat through heat exchanger O 24, go out backflash F 33 group
It is divided into two strands, one enters Ethanol rectification column 9 as overhead reflux, and high-purity is obtained after a stock-traders' know-how heat exchanger P 25 heat exchange
Absolute ethyl alcohol, a bottom of towe component part for Ethanol rectification column 9 returns to Ethanol rectification column 9 after being exchanged heat through heat exchanger Q 26 and is used as bottom of towe
Backflow, another part obtains anhydrous C4 fusels after being exchanged heat through heat exchanger R 27；
The pressure of the Ethanol rectification column 9 is normal pressure, and tower top temperature is 78.5 DEG C, and column bottom temperature is 83 DEG C.
After testing, refined methanol meets GB 338-2011 in the present invention《Industrial methanol》The specification requirements of middle high-class product,
The content of ethanol is more than 99.5% in absolute ethyl alcohol.
A kind of system that refined methanol and absolute ethyl alcohol are extracted from crude carbinol of embodiment 3
As illustrated in fig. 1 and 2, system includes periodic off-gases scrubbing tower 1, pre-rectifying tower 2, compression rectification tower 3, atmospheric distillation tower 4, recovery
Tower 5, fusel oil rectifier 6, membrane filtration dewatering system 7, methanol distillation column 8 and Ethanol rectification column 9；Heat exchanger A 10 passes through pipeline
It is connected with pre-rectifying tower 2, the tower top of pre-rectifying tower 2 is connected by pipeline with heat exchanger B 11, heat exchanger B 11 passes through pipeline point
It is not connected with periodic off-gases scrubbing tower 1 and backflash A 28, the bottom of towe of periodic off-gases scrubbing tower 1 and backflash A 28 bottom pass through pipe
Road is connected with pre-rectifying tower 2, and the bottom of towe of pre-rectifying tower 2 is connected by pipeline through heat exchanger C 12 with compression rectification tower 3, compression rectification
The bottom of towe of tower 3 is connected by pipeline through heat exchanger C12 with atmospheric distillation tower 4, and the tower top of compression rectification tower 4 passes through pipeline and backflash B
29 connections, backflash B 29 is connected with industrial methanol accumulator tank 35 and heat exchanger D 13 respectively by pipeline, and heat exchanger D 13 leads to
Piping is connected with compression rectification tower 3, and the tower top of atmospheric distillation tower 4 is connected by pipeline with heat exchanger E 14, and heat exchanger E 14 leads to
Piping is connected with backflash C 30, backflash C 30 by pipeline respectively with atmospheric distillation tower 4, recovery tower 5 and heat exchanger F
15 are connected, and heat exchanger F 15 is connected by pipeline with industrial methanol accumulator tank 35, and the bottom of towe of atmospheric distillation tower 4 passes through pipeline and heat exchange
Device G 16 is connected, and atmospheric distillation tower 4 is connected by pipeline through feeder trough 34 with recovery tower 5, and the tower top of recovery tower 5 is by pipeline and often
Rectifying column 4 is pressed to be connected, the bottom of towe of recovery tower 5 is connected by pipeline with heat exchanger H 17, and recovery tower 5 is by pipeline through heat exchanger I 18
It is connected with fusel oil rectifier 6, the bottom of towe of fusel oil rectifier 6 is connected by pipeline with heat exchanger K 20, fusel oil rectifier 6
Lower end is connected by pipeline with heat exchanger L 21, and heat exchanger L 21 is connected by pipeline with fusel oil rectifier 6, fusel oil rectifying
The tower top of tower 6 is connected by pipeline through heat exchanger J 19 with backflash D 31, backflash D 31 by pipeline respectively with fusel olein
Evaporate tower 6 with membrane filtration dewatering system 7 to be connected, membrane filtration dewatering system 7 is connected by pipeline with methanol distillation column 8, Methanol Recovery
Tower 8 top is connected by pipeline through heat exchanger M 22 with backflash E 32, backflash E 32 by pipeline respectively with methanol distillation column 8
And atmospheric distillation tower 4 is connected, the bottom of towe of methanol distillation column 8 is connected with heat exchanger N 23 and Ethanol rectification column 9 respectively by pipeline, is changed
Hot device N 23 is connected by pipeline with methanol distillation column 8, and the tower top of Ethanol rectification column 9 is by pipeline through heat exchanger O 24 and backflash
F 33 is connected, and backflash F 33 is connected with Ethanol rectification column 9 and heat exchanger P 25 respectively by pipeline, and heat exchanger P 25 passes through pipe
Road is connected with absolute ethyl alcohol accumulator tank 36, the bottom of towe of Ethanol rectification column 9 by pipeline respectively with heat exchanger Q 26 and heat exchanger R 27
It is connected, heat exchanger Q 26 is connected by pipeline with Ethanol rectification column 9, and heat exchanger R 27 passes through pipeline and anhydrous C4 fusels accumulator tank
37 connections, heat exchanger G 16, heat exchanger H 17, heat exchanger K 20 and membrane filtration dewatering system 7 bottom with waste water system phase
Even.
A kind of system that refined methanol and absolute ethyl alcohol are extracted from crude carbinol of embodiment 4
On the basis of embodiment 3, as depicted in figs. 1 and 2, the membrane filtration dewatering system 7 includes feeder trough A701, superheater
702nd, membrane module 703, water-ring vacuum pump 704, water storage tank 705 and pan tank 706, the feeder trough A 701 are passed through by pipeline
Heat exchanger 1 is connected with superheater 702, and superheater 702 is connected by pipeline with membrane module 703, and membrane module 703 passes through pipeline
It is connected through heat exchanger 2 708 with water storage tank 705, membrane module 703 is connected by pipeline through heat exchanger 3 709 with pan tank 706, water
Storage tank 705 is connected by pipeline with water-ring vacuum pump 704, and parallel way is used between the membrane module 703；The membrane module
703 be inorganic infiltrating and vaporizing membrane.
Claims (9)
1. a kind of technique that refined methanol and absolute ethyl alcohol are extracted from crude carbinol, it is characterised in that comprise the following steps that：
（1）Crude carbinol enters pre-rectifying tower, after the overhead components of pre-rectifying tower exchange heat through heat exchanger B, gas after being exchanged heat through heat exchanger A
Mutually part enters periodic off-gases scrubbing tower, and liquid phase part enters backflash A, and the tower top of periodic off-gases scrubbing tower is fuel gas, bottom of towe group
Divide and enter pre-rectifying tower after the bottom component mixing with backflash A, backflash A top light component is fusel oil；
（2）The bottom of towe component of pre-rectifying tower enters compression rectification tower after being exchanged heat through heat exchanger C, pre-rectifying tower and compression rectification tower are common
With a heat exchanger C；
（3）The overhead components of compression rectification tower are divided into two parts after backflash B, and a part enters after being exchanged heat through heat exchanger D and added
Press rectifying column as backflow, another part as industrial methanol finished product, after the bottom component of compression rectification tower exchanges heat through heat exchanger C
Into atmospheric distillation tower；
（4）The overhead components of atmospheric distillation tower enter backflash C after being exchanged heat through heat exchanger E, are divided into from the backflash C components come out
Three strands, one enter atmospheric distillation tower as overhead reflux, a stock-traders' know-how heat exchanger F heat exchange after as industrial methanol finished product, one
Into recovery tower as overhead reflux, the bottom of towe component of atmospheric distillation tower is discharged into waste water system after being exchanged heat for waste water through heat exchanger G；
（5）The component come out from atmospheric distillation tower enters recovery tower lower end through feeder trough, and the overhead components of recovery tower enter normal pressure
Rectifying column, bottom of towe component are to be discharged into waste water system after waste water exchanges heat through heat exchanger H, and the lower end component of recovery tower is changed through heat exchanger I
Enter fusel oil rectifying column after heat；
（6）The overhead components of fusel oil rectifier enter backflash D after being exchanged heat through heat exchanger J, and the component for going out backflash D is divided into two
Stock, one returns again to fusel oil rectifier and enters membrane filtration as aqueous 10% fusel of being less than of overhead reflux, another stock and be dehydrated and be
System, the bottom of towe component of fusel oil rectifier enters waste water system after being exchanged heat through heat exchanger K, and tower lower end another part is through heat exchanger L
Fusel oil rectifier is returned after heat exchange；
（7）Most of waste water in membrane filtration dewatering system removing fusel, aqueous 0.5% fusel of being no more than enters methanol distillation column；
（8）The overhead components of methanol distillation column are divided into two strands after heat exchanger M and backflash E, and one makees into methanol distillation column
For overhead reflux, the overhead product of another stock and recovery tower enters atmospheric distillation tower, the bottom of towe component one of methanol distillation column together
Part returns to methanol distillation column after being exchanged heat through heat exchanger N and flowed back as bottom of towe, is partly into Ethanol rectification column as ethanol essence
Evaporate the charging of tower；
（9）The overhead components of Ethanol rectification column enter backflash F after being exchanged heat through heat exchanger O, and the component for going out backflash F is divided into two
Stock, one enters Ethanol rectification column as overhead reflux, the absolute ethyl alcohol of high-purity, second is obtained after stock-traders' know-how heat exchanger P heat exchange
A bottom of towe component part for alcohol rectifying column returns to Ethanol rectification column after being exchanged heat through heat exchanger Q and flowed back as bottom of towe, another part warp
Anhydrous C4 fusels are obtained after heat exchanger R heat exchange.
2. technique according to claim 1, it is characterised in that the step（1）Described in pre-rectifying tower tower top pressure be
139 kPaA, temperature is 74.8 DEG C；Tower bottom pressure is that 147 kPaA temperature are 77.5 DEG C, and reflux ratio is 0.92；Periodic off-gases are washed
The temperature of the pressure normal pressure of tower, tower top and bottom of towe is that desalination water spray system is provided with normal temperature, periodic off-gases scrubbing tower, positioned at gas phase
Entrance top；
The step（2）Described in compression rectification tower tower top pressure be 800 kPaA, temperature be 128 DEG C；Tower bottom pressure is 813
KPaA, temperature is 134 DEG C；Reflux ratio is 3.0；
The step（4）Described in atmospheric distillation tower tower top pressure be 113 kPaA, temperature be 67.5 DEG C；Tower bottom pressure is
143 kPaA, temperature is 110 DEG C；Reflux ratio is 1.85；
The step（5）Described in recovery tower tower top pressure be 133 kPaA, temperature be 72 DEG C；Tower bottom pressure is 153
KPaA, temperature is 111.5 DEG C；Capacity of returns 3100kg/h；
The step（6）Described in fusel oil rectifier tower top pressure be 23 kPaA, temperature be 99.45 DEG C；Tower bottom pressure is
30 kPaA, temperature is 100 DEG C；Reflux ratio is 12-13；
The step（8）Described in methanol distillation column pressure be normal pressure, tower top temperature be 69 DEG C, column bottom temperature be 79 DEG C；
The step（9）Described in Ethanol rectification column pressure be normal pressure, tower top temperature be 78.5 DEG C, column bottom temperature be 83 DEG C.
3. technique according to claim 1, it is characterised in that the step（6）Middle reflux ratio is 12.5.
4. the technique according to claim any one of 1-3, it is characterised in that the step（7）Middle membrane filtration dewatering system
Including feeder trough A, superheater, membrane module, water-ring vacuum pump, water storage tank and pan tank, the feeder trough A is by pipeline through changing
Hot device one is connected with superheater, and superheater is connected by pipeline with membrane module, and membrane module is stored up by pipeline through heat exchanger two and water
Tank is connected, and membrane module is connected by pipeline through heat exchanger three with pan tank, and water storage tank is connected by pipeline with vavuum pump.
5. the technique according to claim any one of 1-3, it is characterised in that the pre-rectifying tower, compression rectification tower, normal pressure
Rectifying column, recovery tower, fusel oil rectifier, methanol distillation column and Ethanol rectification column add column plate using plate column or structured packing
Combination tower.
6. technique according to claim 5, it is characterised in that the pre-rectifying tower, compression rectification tower, atmospheric distillation tower,
Recovery tower, fusel oil rectifier, methanol distillation column and Ethanol rectification column are the combination tower of structured packing plus column plate.
7. a kind of system that refined methanol and absolute ethyl alcohol are extracted from crude carbinol, it is characterised in that system is washed including periodic off-gases
Tower, pre-rectifying tower, compression rectification tower, atmospheric distillation tower, recovery tower, fusel oil rectifier, membrane filtration dewatering system, Methanol Recovery
Tower and Ethanol rectification column；Heat exchanger A is connected by pipeline with pre-rectifying tower, and the tower top of pre-rectifying tower passes through pipeline and heat exchanger B
Connection, heat exchanger B is connected with periodic off-gases scrubbing tower and backflash A respectively by pipeline, the bottom of towe of periodic off-gases scrubbing tower and backflow
Groove A bottom is connected by pipeline with pre-rectifying tower, and pre-rectifying tower bottom of towe is by pipeline through heat exchanger C and compression rectification tower phase
Even, compression rectification tower bottom of towe is connected by pipeline through heat exchanger C with atmospheric distillation tower, and compression rectification column overhead is by pipeline with returning
Chute B connections, backflash B is connected with industrial methanol accumulator tank and heat exchanger D respectively by pipeline, heat exchanger D by pipeline with
Compression rectification tower is connected, and atmospheric distillation column overhead is connected by pipeline with heat exchanger E, and heat exchanger E passes through pipeline and backflash C phases
Even, backflash C is connected with atmospheric distillation tower, recovery tower and heat exchanger F respectively by pipeline, and heat exchanger F passes through pipeline and industry
Methanol accumulator tank is connected, and atmospheric distillation tower bottom of towe is connected by pipeline with heat exchanger G, and atmospheric distillation tower is by pipeline through feeder trough
It is connected with recovery tower, reclaims column overhead and be connected by pipeline with atmospheric distillation tower, recovery tower bottom of towe passes through pipeline and heat exchanger H phases
Even, recovery tower is connected by pipeline through heat exchanger I with fusel oil rectifier, and the bottom of towe of fusel oil rectifier passes through pipeline and heat exchange
Device K is connected, and fusel oil rectifier lower end is connected by pipeline with heat exchanger L, and heat exchanger L passes through pipeline and fusel oil rectifier phase
Even, fusel oil rectifying column tower top is connected by pipeline through heat exchanger J with backflash D, backflash D by pipeline respectively with fusel oil
Rectifying column is connected with membrane filtration dewatering system, and membrane filtration dewatering system is connected by pipeline with methanol distillation column, methanol distillation column
Top be connected by pipeline through heat exchanger M with backflash E, backflash E by pipeline respectively with methanol distillation column and atmospheric distillation tower
It is connected, methanol distillation column bottom of towe is connected with heat exchanger N and Ethanol rectification column respectively by pipeline, and heat exchanger N passes through pipeline and first
Alcohol recovery tower is connected, and Ethanol rectification column tower top is connected by pipeline through heat exchanger O with backflash F, and backflash F is distinguished by pipeline
It is connected with Ethanol rectification column and heat exchanger P, heat exchanger P is connected by pipeline with absolute ethyl alcohol accumulator tank, Ethanol rectification column bottom of towe
It is connected respectively with heat exchanger Q and heat exchanger R by pipeline, heat exchanger Q is connected by pipeline with Ethanol rectification column, heat exchanger R leads to
Piping is connected with anhydrous C4 fusels accumulator tank, heat exchanger G, heat exchanger H, heat exchanger K and membrane filtration dewatering system bottom it is equal
It is connected with waste water system.
8. system according to claim 7, it is characterised in that the membrane filtration dewatering system includes feeder trough A, overheat
Device, membrane module, vavuum pump, water storage tank and pan tank, the feeder trough A are connected by pipeline through heat exchanger one with superheater, mistake
Hot device is connected by pipeline with membrane module, and membrane module is connected by pipeline through heat exchanger two with water storage tank, and membrane module passes through pipeline
It is connected through heat exchanger three with pan tank, water storage tank is connected by pipeline with vavuum pump.
9. system according to claim 8, it is characterised in that series, parallel or series connection are used between the membrane module
The mode of parallel connection mixing；The vavuum pump is water-ring vacuum pump；The membrane module is inorganic infiltrating and vaporizing membrane.
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| CN110759812A (en) * | 2019-11-12 | 2020-02-07 | 陕西聚能新创煤化科技有限公司 | Recovery method and recovery system of fusel ethanol in methanol rectification process |
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