CN110327647A - A kind of refining crude methanol process of three tower triple effect of modified - Google Patents
A kind of refining crude methanol process of three tower triple effect of modified Download PDFInfo
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- CN110327647A CN110327647A CN201910655239.5A CN201910655239A CN110327647A CN 110327647 A CN110327647 A CN 110327647A CN 201910655239 A CN201910655239 A CN 201910655239A CN 110327647 A CN110327647 A CN 110327647A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- 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
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
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Abstract
The present invention provides a kind of refining crude methanol process of three tower triple effect of modified, including pre-rectifying tower, first rectifying column and Second distillation column, so that the heat of the refined methanol gas phase of first rectifying column overhead extraction is met Second distillation column tower bottom first and boils load again, then the refined methanol gas phase cocurrent of fixed gas phase after heat exchange and Second distillation column overhead extraction separates one its heat is made to meet pre-rectifying tower tower bottom and boils load again.The present invention can further decrease system energy consumption, and reduce by three tower loads, avoid the transformation to traditional three tower methanol rectification process systems difficult.
Description
Technical field
The invention belongs to chemical materials purification process and equipment technical fields, and in particular to a kind of improved crude carbinol
Refining methd and system.
Background technique
Crude carbinol rectifying is to obtain the common process method of high-purity methanol product at present, generallys use three tower methanol essence of tradition
(fair current double-effect rectification) technique is evaporated, i.e. crude carbinol sequence passes through pre-rectifying tower, compression rectification tower, atmospheric distillation tower progress rectifying point
From.For the energy consumption for reducing methanol rectification, applicant proposed a kind of refining crude methanol process of three tower triple effects in 2018, makes
The refined methanol gas phase heat of compression rectification column overhead extraction meets atmospheric distillation tower bottom first and boils load, remaining refined methanol gas phase again
Heat boils again for pre-rectifying tower tower bottom provides partial heat.The distribution of two parts heat enables to compression rectification column overhead gas phase
The heat of material is obtained an equitable breakdown and is utilized, and reduces system energy consumption.But this process still has some shortcomings, a side
The heat of face, atmospheric distillation tower and pre-rectifying tower tower bottom reboiler is all provided by compression rectification column overhead gas phase, leads to pre- essence
Evaporating tower tower bottom reboiler institute calorific requirement may be insufficient, and heat-exchange capacity is limited, and on the other hand, compression rectification tower tower load may increase
Add, higher requirement proposed to the compatibilization ability of compression rectification tower, but in existing factory pressurizing tower compatibilization ability it is limited, it is difficult
To meet the needs required increase-volume.These deficiencies make the refining crude methanol process of this three towers triple effect in system energy consumption
It reduces the effect that aspect can play to be limited, comprehensive energy consumption reduces limited.
Summary of the invention
The purpose of the present invention is to provide a kind of refining crude methanol processes of three tower triple effect of modified, can be further
System energy consumption is reduced, and reduces by three tower loads, avoids the transformation to traditional three tower methanol rectification process systems difficult.
The refining crude methanol process of three tower triple effect of modified of the invention, including pre-rectifying tower, first rectifying column and
Second distillation column, make the heat of the refined methanol gas phase of first rectifying column overhead extraction meet first Second distillation column tower bottom boil again it is negative
Lotus, the refined methanol gas phase cocurrent of fixed gas phase and Second distillation column overhead extraction after heat exchange, then separating one makes its heat
Amount meets pre-rectifying tower tower bottom and boils load again.
Above-mentioned process route enables the tower top heat of first rectifying column to be utilized twice, respectively provides the second essence
Evaporate the net quantity of heat and the partial heat of pre-rectifying tower tower bottom reboiler is provided that tower tower bottom is boiled again.Simultaneously as the first rectifying
The refined methanol gas phase fixed gas phase after the heat exchange of column overhead extraction and the refined methanol gas phase of Second distillation column overhead extraction are simultaneously
Stream, so that the tower top heat of Second distillation column also can make full use of and effectively be supplemented insufficient heat, further mentions
Heating efficiency in high system, while the heat supply load of first rectifying column is effectively reduced, reduce to the first rectifying
The requirement of tower increase-volume demand.Boiling hot amount is provided first rectifying column tower bottom by external steam again, therefore the above-mentioned process route of this case can
To realize that the triple effect of external steam heat utilizes: external steam heat is initially used for first rectifying column tower bottom and boils again, is considered as an effect；
The amount boiling hot again that first rectifying column obtains is transferred to top gaseous phase by reaction in tower, then is used for Second distillation column by top gaseous phase
Tower bottom is boiled again, is considered as two effects；Two effects mutually continue on for pre-rectifying tower tower bottom using fixed gas after heat transmitting and boil again, are considered as triple effect.
Using heat efficiency is played to the greatest extent, the system that effectively reduces totally needs to disappear the above-mentioned triple effect to external steam
The amount of steam is consumed, system energy consumption is saved.
Specifically, light component and a small amount of gaseous methanol contain from pre-rectifying tower overhead extraction after crude carbinol enters pre-rectifying tower
Water methanol solution A produces from pre-rectifying tower tower bottom and enters first rectifying column；The refined methanol gas phase of first rectifying column overhead extraction
Material is sent into Second distillation column tower bottom and provides again boiling hot amount for Second distillation column, and the material after carrying out heat exchange is divided at least
Three strands: first strands are used as phegma to flow back into first rectifying column, and second strand produces as product, and third stock is as fixed gas phase
With the refined methanol gas phase cocurrent of Second distillation column overhead extraction；First rectifying column tower bottom produces aqueous methanol solution B and enters second
Rectifying column；The refined methanol gaseous phase materials of Second distillation column overhead extraction and above-mentioned conduct after boiling hot amount is provided again for Second distillation column
After the material cocurrent of third stock fixed gas phase, it is again split into three strands: first strands and send to pre-rectifying tower tower bottom and mentioned for pre-rectifying tower
For boiling hot amount again, second strand becomes phegma and flows back into Second distillation column, and third stock is produced as product；Second distillation column tower
Bottom extracted waste water material, side take-off fusel material.
Wherein, the pre-rectifying tower tower bottom has at least two reboiling devices, preferably three, wherein a reboiling device
It is exchanged with wherein one progress heat of the refined methanol gaseous phase materials of Second distillation column overhead extraction, other reboiling devices and outside
Steam carries out heat exchange (i.e. its boiling hot amount is provided by external steam again).When system is driven, due to shortage of heat in system,
Boiling hot amount is mainly provided by external steam pre-rectifying tower tower bottom again, after system even running, pre-rectifying tower tower bottom boiling hot amount again
It can be provided completely by the refined methanol gaseous phase materials of Second distillation column overhead extraction.
Wherein, the refined methanol gaseous phase materials of the Second distillation column overhead extraction are not boiled to the offer of pre-rectifying tower tower bottom again
The part of heat, after first passing around condensation, is re-used as liquid phase material and is handled, that is, respectively becomes above-mentioned second burst of reflux
Liquid and third stock product.
Wherein, the Second distillation column middle and lower part, which also produces, fusel, and aqueous fusel is 65-76w%, and the temperature of extraction is
105-122 DEG C, pressure 170-265kPa.The design of fusel extraction route advantageously reduces the second atmospheric distillation tower load, mentions
High methanol purification efficiency, further decreases energy consumption, and fusel after the recovery can also obtain resource utilization benefit after further treatment
With.
Tower bottom boils the needs of load again in overhead extraction gas relative system to meet first rectifying column and Second distillation column,
Three Deethanizer design pressure can use two kinds of combinations:
Mode one: pre-rectifying tower is atmospheric operation, and first rectifying column is pressurized operation, and Second distillation column is pressurized operation,
The operating pressure of first rectifying column is higher than the operating pressure of Second distillation column, and the operation pressure of first rectifying column and Second distillation column
Power is above conventional design pressure.Specifically, three Deethanizer design pressure are preferably that pre-rectifying tower operating pressure is 103-160kPa,
First rectifying column operating pressure is 790-1100kPa, and Second distillation column operating pressure is 180-350kPa.
Mode two: pre-rectifying tower is decompression operation, and first rectifying column is pressurized operation, and Second distillation column is pressurized operation,
The operating pressure of first rectifying column is higher than the operating pressure of Second distillation column, and the operating pressure of Second distillation column is higher than conventional set
Count pressure but lower than the operating pressure of Second distillation column in mode one.Specifically, three Deethanizer design pressure are preferably pre-rectifying tower
Operating pressure is 40-92kPa, and first rectifying column operating pressure is 650-1150kPa, and Second distillation column operating pressure is 150-
220kPa。
The optimal control of process conditions makes in the case where guaranteeing refined methanol purity, and system energy consumption advanced optimizes drop
It is low.Therefore, this case optimizes the process regulation parameter of three towers:
For mode one: the number of plates of the pre-rectifying tower is 50-58 layers, and the temperature of overhead extraction is 60-65.2 DEG C, presses
Power is 110-130kPa, reflux ratio 3.5-4.8, and it is 75-85 DEG C that tower bottom, which produces temperature, pressure 136-160kPa；Described
The number of plates of one rectifying column is 70-95 layers, and the temperature of overhead extraction is 115-145 DEG C, pressure 890-1050kPa, reflux ratio
For 1.5-2.9, it is 145-155 DEG C that tower bottom, which produces temperature, pressure 950-1045kPa；The number of plates of the Second distillation column is
85-95 layers, the temperature of overhead extraction is 70-105 DEG C, pressure 180-260kPa, reflux ratio 1.3-2.2, tower bottom extraction temperature
Degree is 115-129 DEG C, pressure 220-290kPa.
For mode two: the number of plates of the pre-rectifying tower is 45-58 layers, and the temperature of overhead extraction is 42-49 DEG C, pressure
For 50-60kPa, reflux ratio 2.5-4.6, it is 55-68 DEG C that tower bottom, which produces temperature, pressure 70-92kPa；First rectifying
The number of plates of tower is 70-95 layers, and the temperature of overhead extraction is 105-132 DEG C, pressure 690-742kPa, reflux ratio 1.4-
2.9, it is 125-145 DEG C that tower bottom, which produces temperature, pressure 720-815kPa；The number of plates of the Second distillation column is 85-95 layers,
The temperature of overhead extraction is 65-85 DEG C, pressure 150-210kPa, reflux ratio 1.4-2.9, and it is 110- that tower bottom, which produces temperature,
120 DEG C, pressure 150-195kPa.
Wherein, the gaseous phase materials of the pre-rectifying tower overhead extraction are successively condensed by condensation for the first time and second, the
Condensation liquid phase after time condensation carries out gas-liquid separation, the isolated separating liquid of the gentle liquid of condensation liquid phase through condensing for the first time
Phase cocurrent flows back into pre-rectifying tower as phegma, and a small amount of fixed gas returns to second of condensation operation after cocurrent, through second
The isolated separation gas phase of the fixed gas phase and gas-liquid of condensation carries out subsequent processing (handling as entered flare system).Using two
Secondary condensation can be improved condensing recovery efficiency, reduce the turnover rate of methanol.The design can be able to satisfy pre-rectifying tower and design in normal pressure
In operation, the operation including the operating condition in aforesaid way one.
Further, for needing the pre-rectifying tower of decompression operation, can further make described not coagulate through what is condensed for the second time
Gas phase carries out gas-liquid separation together with through second of condensed condensation liquid phase after condensing using third time, and gas-liquid separation obtains
Separation gas phase carry out subsequent processing after the 4th condensation, and by the 4th condensed material via vacuum pump again into
Enter subsequent processing, the vacuum pump is parallel with regulating valve；Wherein, the third time is condensed into room temperature condensation, is condensed into for the 4th time
Cryogenic condensation.The third time condensation and the 4th adding for condensation can not only further increase condensing recovery efficiency, and
Pre-rectifying tower tower top pressure can be reduced by the connection of vacuum pump, so that the pre-rectifying tower of atmospheric operation is improved to can be into
Row decompression operation, the operating condition operation being effectively applicable in aforesaid way two require.In addition, the design can also be by regulating valve
The intensity of vacuum pump is adjusted, or completely closes vacuum pump, is allowed in the case where not playing a role, allows pre-rectifying tower
The condition for restoring atmospheric operation, i.e., can also meet the operation of operating condition in aforesaid way one simultaneously.
In addition, the feed composition of the crude carbinol can be with are as follows: methanol content 50-97w%, light component impurity 1.5-
2.5w%, heavy constituent impurity 7.5-13.5w%；Methanol content is 18- in the gaseous phase materials of the pre-rectifying tower overhead extraction
Methanol content is 70-85w% in 28w%, the aqueous methanol solution A of tower bottom extraction；The first rectifying column tower bottom extraction contains
Methanol content is 50-75w% in water methanol solution B.The optimal control of every input and output material composition is made to guarantee that refined methanol is pure
While degree, reduction energy consumption, additionally it is possible to optimize purification efficiency.
Compared with prior art, present invention has the advantage that
(1) it can be realized the secondary use to the first pressurization column overhead heat, and form the triple effect thermal energy to external steam
It utilizes, utilization efficiency of heat energy greatly improves, and the energy consumption of methanol fractionation system is effectively reduced.Compared to published common three tower three
Rectification process (heat of atmospheric distillation tower and pre-rectifying tower tower bottom reboiler is all provided by compression rectification column overhead gas phase) is imitated,
The integral load of first rectifying column is made full use of while being significantly reduced in thermal energy, improves the heat capacity of preheating.
(2) in present invention process, refined methanol comprehensive energy consumption per ton can be reduced to 0.71 ton of steam, compared to published
0.85-0.90 tons of steam consumption of common three towers three-effect rectification technique, steam consumption reduces 24.1%.
(3) since the compatibilization ability of the pressurizing tower of different factories is different, the tower diameters of some equipment, reboiler heat exchange area by
To limitation, tower internals gas-liquid flux is limited, it has been disclosed that common three towers three-effect rectification process route modification scheme enforcement difficulty compared with
Greatly.The present invention compares traditional three tower fair current economic benefits and social benefits techniques and common three towers three-effect rectification technique, avoids proposing first rectifying column
Scrap build can be realized by adding the simple devices such as reboiler, condenser, vacuum pump in biggish capacity-increasing transformation demand, can
To substantially reduce new process project transformation enforcement difficulty, and various working preferably is adapted to simultaneously, effectively promotes existing factory
Energy-saving horizontal.
Detailed description of the invention
The attached drawing for constituting a part of the invention is used to provide further understanding of the present invention, schematic reality of the invention
It applies example and its explanation is used to explain the present invention, do not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 is the process flow chart of the embodiment of the present invention 1.
Fig. 2 is the process flow chart of the embodiment of the present invention 2.
Wherein thick blue line is based on liquid phase process logistics, and fine powder colo(u)r streak is based on gaseous process stream.
Specific embodiment
In order to better understand the present invention, below with reference to specific attached drawing, the present invention will be described in detail.In order to explain in detail
The present invention is stated, example below has carried out the explanation of many process details, is not intended to cause the present invention improper restriction.
Embodiment 1 (mode one)
As shown in Figure 1, crude carbinol (40 DEG C, 0.5MPa, 120m3/ h, material R1) enter in advance through the first preheater M4 preheating
In rectifying column M1, come into full contact with by the gas-liquid of 52 layers in tower efficient DVST column plate or several segments filler, it is light in crude carbinol
Component and a small part methanol are in a gaseous form from methanol content in pre-rectifying tower M1 overhead extraction, the gaseous phase materials of overhead extraction
About 22%, the temperature of overhead extraction is 62.9 DEG C, and pressure 119kPa, it is cold that the gaseous phase materials of overhead extraction sequentially enter first
Condenser M5 and the second condenser M6 carries out time condensation, and the condensate liquid after time condensation enters gas-liquid separator M7, after separation
Fixed gas (CO, CO2、H2、N2、CH4, more carbon alkanes, ethyl acetate, 40 DEG C, 0.12MPa, 3.0-50.0m such as dimethyl ether3/h)
It is combined into subsequent post-processing and flare system with the second condensed fixed gas of condenser M6, after gas-liquid separator M7 separation
Condensate liquid and the first condensed condensate liquid of condenser M5 enter liquid conduct in the first return tank M8, the first return tank M8
52 layers of the top column plate that phegma enters pre-rectifying tower M1 flows back, the drag-outs that reflux ratio controls methanol for 4.0, and first
A small amount of fixed gas in return tank M8, which backs into the second condenser M6, to be continued to condense.
The bottom the pre-rectifying tower M1 is parallel at least two reboilers, and this example is three, respectively reboiler M9, boils again
Device M10 and reboiler M11.Reboiler M9 and reboiler M11 passes through external steam pipeline respectively and carries out conventional heat supply.Wherein one
The platform side reboiler M11 be equipped with surge tank M12, from the gaseous phase materials of Second distillation column M3 overhead extraction one (about 95 DEG C,
99.95% methanol, 0.26Mpa, material R5) enter surge tank M12, then thermal coupling (heat exchange) is carried out with reboiler M11
Cooling forms lime set, and lime set returns to the third return tank M21 of Second distillation column M3.
The pre-rectifying tower M1 tower bottom produces aqueous methanol solution A (material R2), and wherein methanol content is about 83%, tower bottom
The temperature of extraction is 80 DEG C, pressure 1.41kg/cm2.Aqueous methanol solution A enters the after the second preheater M13 preheating
On the middle and lower part column plate of one rectifying column M2,125 DEG C of feeding temperature.The bottom the first rectifying column M2 is parallel at least one again
Device is boiled, this example is two, and respectively reboiler M14 and reboiler M15, the two pass through external steam pipeline respectively and carries out heat supply.
Gas-liquid carries out gas-liquid mass transfer, heat transfer, the refined methanol that tower top comes out by efficient DVST column plate or filler in first rectifying column M2
(135 DEG C, 99.98% methanol, 0.9902Mpa, material R4) enter Second distillation column M3 tower bottom reboiler M19 shell side into
Row heat exchange, the condensate liquid after refined methanol heat exchange return to the second return tank M16.Refined methanol lime set material in second return tank M16
It is divided into the 1st layer of the top column plate that two strands: first strands enter first rectifying column M2 to flow back, reflux ratio 2.2；Second strand successively
Enter product storage tank after the first cooler M17 and the second cooler M18 carries out secondary cooling；Essence in second return tank M16
The refined methanol gas phase cocurrent of methanol fixed gas and Second distillation column M3 overhead extraction.
The first rectifying column M2 tower bottom produces aqueous methanol solution B (material R3), and wherein methanol content is about 70%, tower
The temperature of bottom extraction is 145 DEG C, pressure 10.45kg/cm2.Aqueous methanol solution B enters the middle and lower part tower of Second distillation column M3
On plate, 145 DEG C of feeding temperature.In Second distillation column M3, gas-liquid carries out gas-liquid heat-transfer by high-efficient tower plate or filler, passes
Matter, moisture, ethyl alcohol, fusel etc. in methanol are sufficiently removed.The gaseous phase materials of Second distillation column M3 overhead extraction are smart first
The pressure of alcohol (99.95% methanol, material R6) overhead extraction is 2.1kg/cm2.The refined methanol material and the second return tank M16
In refined methanol fixed gas cocurrent after, be divided into two strands: one (material R5) enter surge tank M12, then with reboiler M11 carry out
Lime set is formed after thermal coupling and returns to third return tank M21, also enters third return tank after the 5th condenser M20 of stock-traders' know-how condensation
M21.Material in third return tank M21 is also classified into two strands: one the 1st layer of top column plate for returning to Second distillation column M3 is returned
Stream, reflux ratio 1.95, enter product storage tank after another stock-traders' know-how third cooler M22 is cooling by 90 DEG C of phegma temperature.
The middle and lower part Second distillation column M3 is equipped with fusel (material R8) and produces mouth, and the fusels such as ethyl alcohol of enrichment pass sequentially through the
(40 DEG C, 70% water, 0.167Mpa) the feeding fusel tank fields five cooler M23 and the second surge tank M24.
Second distillation column M3 tower bottom extracted waste water material (material R7), methanol content at least reduce to 0.1% hereinafter, tower bottom
The temperature of extraction is 124 DEG C, pressure 2.3kg/cm2, after the 4th cooler M25 is cooling, it is transported to subsequent waste disposal system
System is handled.
In above-mentioned technical process, the composition of correlative is as shown in table 1.
1 material of table forms unit w%
Using the above scheme, certain 600,000 tons/year of refining crude methanol producer is transformed, the charging of 96.7t/h crude carbinol.Change
Refined methanol purity is 99.9% before making, system energy consumption 56.85MKcal/h, and methanol produced quantity is 84.1t/h, single ton of refined methanol
Steam consumption be 1.37.Refined methanol purity is methanol 99.95%, system energy consumption 30.61MKcal/h, methanol after transformation
Produced quantity is 84.1t/h, and the steam consumption of single ton of refined methanol is 0.727.Compared to traditional handicraft, system energy consumption is reduced
46.9%.
Embodiment 2 (mode two)
As shown in Fig. 2, crude carbinol (40 DEG C, 0.5MPa, 120m3/ h, material R1) enter in advance through the first preheater M4 preheating
In rectifying column M1, come into full contact with by the gas-liquid of 52 layers in tower efficient DVST column plate or several segments filler, it is light in crude carbinol
Component and a small part methanol are in a gaseous form from methanol content in pre-rectifying tower M1 overhead extraction, the gaseous phase materials of overhead extraction
About 28%, the temperature of overhead extraction is 48 DEG C, and pressure 60kPa, the gaseous phase materials of overhead extraction sequentially enter the first condensation
Device M5 and the second condenser M6 carries out time condensation, and the condensate liquid after time condensation enters gas-liquid separator M7, through secondary cold
Fixed gas after solidifying enters gas-liquid separator M7 through third condenser M26, the fixed gas after being separated in gas-liquid separator M7 into
Enter the 4th condenser M27, the flare system of subsequent processing is then sent into through a vacuum pump M28, is parallel on the vacuum pump M28
Regulating valve M29, for adjusting vacuum pump M28 mass flow, fixed gas (CO, CO for being come out from vacuum pump M282、H2、N2、CH4、
40 DEG C of more carbon alkanes, ethyl acetate, dimethyl ether etc., 0.12MPa, 3.0-50.0m3/ h) enter subsequent post-processing flare system.
Condensate liquid and the first condensed condensate liquid of condenser M5 after gas-liquid separator M7 separation enter the first return tank M8, the
52 layers of the top column plate that liquid enters pre-rectifying tower M1 as phegma in one return tank M8 flows back, reflux ratio 4.1
The drag-out for controlling methanol, a small amount of fixed gas in the first return tank M8 back into the second condenser M6 continue it is cold
It is solidifying.
The bottom the pre-rectifying tower M1 is parallel at least two reboilers, and this example is three, respectively reboiler M9, boils again
Device M10 and reboiler M11.Reboiler M9 and reboiler M11 passes through external steam pipeline respectively and carries out conventional heat supply.Wherein one
The platform side reboiler M11 be equipped with surge tank M12, from the gaseous phase materials of Second distillation column M3 overhead extraction one (about 80 DEG C,
99.96% methanol, 0.17Mpa, material R5) enter surge tank M12, then thermal coupling (heat exchange) is carried out with reboiler M11
Cooling forms lime set, and lime set returns to the third return tank M21 of Second distillation column M3.
The pre-rectifying tower M1 tower bottom produces aqueous methanol solution A (material R2), and wherein methanol content is about 84%, tower bottom
The temperature of extraction is 62.8 DEG C, pressure 0.82kg/cm2.Aqueous methanol solution A enters after the second preheater M13 preheating
On the middle and lower part column plate of first rectifying column M2,122 DEG C of feeding temperature.The bottom the first rectifying column M2 is parallel at least one
Reboiler, this example are two, and respectively reboiler M14 and reboiler M15, the two pass through external steam pipeline respectively and supplied
Heat.Gas-liquid carries out gas-liquid mass transfer, heat transfer, the refined methanol that tower top comes out by efficient DVST column plate or filler in first rectifying column M2
(122 DEG C, 99.99% methanol, 0.702Mpa, material R4) enter Second distillation column M3 tower bottom reboiler M19 shell side into
Row heat exchange, the condensate liquid after refined methanol heat exchange return to the second return tank M16.Refined methanol lime set material in second return tank M16
It is divided into the 1st layer of the top column plate that two strands: first strands enter first rectifying column M2 to flow back, reflux ratio 2.2；Second strand successively
Enter product storage tank after the first cooler M17 and the second cooler M18 carries out secondary cooling；Essence in second return tank M16
The refined methanol gas phase cocurrent of methanol fixed gas and Second distillation column M3 overhead extraction.
The first rectifying column M2 tower bottom produces aqueous methanol solution B (material R3), and wherein methanol content is about 73%, tower
The temperature of bottom extraction is 133 DEG C, pressure 7.85kg/cm2.Aqueous methanol solution B enters the middle and lower part tower of Second distillation column M3
On plate, 132 DEG C of feeding temperature.In Second distillation column M3, gas-liquid carries out gas-liquid heat-transfer by high-efficient tower plate or filler, passes
Matter, moisture, ethyl alcohol, fusel etc. in methanol are sufficiently removed.The gaseous phase materials of Second distillation column M3 overhead extraction are smart first
The pressure of alcohol (99.96% methanol, material R6) overhead extraction is 1.56kg/cm2.The refined methanol material and the second return tank
After refined methanol fixed gas cocurrent in M16, be divided into two strands: one (material R5) enter surge tank M12, then with reboiler M11
Lime set return third return tank M21 is formed after carrying out thermal coupling, the 5th condenser M20 of a stock-traders' know-how also enters third after condensing and flows back
Tank M21.Material in third return tank M21 is also classified into two strands: one the 1st layer of top column plate for returning to Second distillation column M3 carries out
Reflux, reflux ratio 1.9, phegma temperature 70 C enter product storage tank after another stock-traders' know-how third cooler M22 is cooling.
The middle and lower part Second distillation column M3 is equipped with fusel (material R8) and produces mouth, and the fusels such as ethyl alcohol of enrichment pass sequentially through the
(40 DEG C, 70% water, 0.197Mpa) the feeding fusel tank fields five cooler M23 and the second surge tank M24.
Second distillation column M3 tower bottom extracted waste water material (material R7), methanol content at least reduce to 0.1% hereinafter, tower bottom
The temperature of extraction is 115 DEG C, pressure 1.75kg/cm2, after the 4th cooler M25 is cooling, it is transported to subsequent waste disposal system
System is handled.
In above-mentioned technical process, the composition of correlative is as shown in table 2.
2 material of table forms unit w%
Using the above scheme, certain 600,000 tons/year of refining crude methanol producer is transformed, the charging of 96.72t/h crude carbinol.
Refined methanol purity is 99.92% before being transformed, system energy consumption 56.85MKcal/h, and methanol produced quantity is 84.1t/h, single ton of smart first
The steam consumption of alcohol is 1.37.Refined methanol purity is methanol 99.98%, system energy consumption 31.76MKcal/h, first after transformation
Alcohol produced quantity is 83.9t/h, and the steam consumption of single ton of refined methanol is 0.735.Compared to traditional handicraft, system energy consumption is reduced
46.3%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of refining crude methanol process of three tower triple effect of modified, including pre-rectifying tower, first rectifying column and the second essence
Tower is evaporated, so that the heat of the refined methanol gas phase of first rectifying column overhead extraction is met Second distillation column tower bottom first and boils load again, heat
The refined methanol gas phase cocurrent of fixed gas phase and Second distillation column overhead extraction after exchange, then separating one meets its heat
Pre-rectifying tower tower bottom boils load again.
2. the refining crude methanol process of three tower triple effect of modified according to claim 1, which is characterized in that including under
State step: after crude carbinol enters pre-rectifying tower, from pre-rectifying tower overhead extraction, aqueous methanol is molten for light component and a small amount of gaseous methanol
Liquid A is produced from pre-rectifying tower tower bottom and is entered first rectifying column；The refined methanol gaseous phase materials of first rectifying column overhead extraction are sent into
Second distillation column tower bottom simultaneously provides again boiling hot amount for Second distillation column, and the material after carrying out heat exchange is divided at least three strands: the
One flows back into first rectifying column as phegma, and second strand produces as product, and third stock is as fixed gas phase and second
The refined methanol gas phase cocurrent of the top of the distillation column extraction；First rectifying column tower bottom extraction aqueous methanol solution B enters Second distillation column；
The refined methanol gaseous phase materials of Second distillation column overhead extraction and above-mentioned provide again for Second distillation column are used as third stock after boiling hot amount
After the material cocurrent of fixed gas phase, it is again split into three strands: first strands and send to pre-rectifying tower tower bottom and being provided for pre-rectifying tower and boil again
Heat, second strand becomes phegma and flows back into Second distillation column, and third stock is produced as product；The extraction of Second distillation column tower bottom
Waste water material, side take-off fusel material.
3. the refining crude methanol process of three tower triple effect of modified according to claim 1, which is characterized in that described pre-
Rectifying tower bottom has at least two reboiling devices, preferably three, wherein a reboiling device is adopted with Second distillation column tower top
Wherein one progress heat exchange of refined methanol gaseous phase materials out, other reboiling devices carry out heat with external steam and exchange.
4. the refining crude methanol process of three tower triple effect of modified according to claim 1, which is characterized in that described
The refined methanol gaseous phase materials of two the top of the distillation column extraction, do not provide again the part of boiling hot amount to pre-rectifying tower tower bottom, first pass around
After condensation, it is re-used as liquid phase material and is handled.
5. the refining crude methanol process of three tower triple effect of modified according to claim 1, which is characterized in that described
Two rectifying column middle and lower parts, which also produce, fusel, and aqueous fusel is 65-76w%, and the temperature of extraction is 105-122 DEG C, and pressure is
170-265kPa。
6. the refining crude methanol process of three tower triple effect of modified according to claim 1, which is characterized in that three towers are set
Pressure is counted using one of following two ways:
Mode one: pre-rectifying tower is atmospheric operation, and first rectifying column is pressurized operation, and Second distillation column is pressurized operation, first
The operating pressure of rectifying column is higher than the operating pressure of Second distillation column, and first rectifying column and the operating pressure of Second distillation column are equal
Higher than conventional design pressure；
Mode two: pre-rectifying tower is decompression operation, and first rectifying column is pressurized operation, and Second distillation column is pressurized operation, first
The operating pressure of rectifying column is higher than the operating pressure of Second distillation column, and the operating pressure of Second distillation column is higher than conventional design pressure
Power but the operating pressure for being lower than Second distillation column in mode one.
7. the refining crude methanol process of three tower triple effect of modified according to claim 6, which is characterized in that
It is preferably that pre-rectifying tower operating pressure is 103-160kPa, first rectifying column operation for one: three Deethanizer design pressure of mode
Pressure is 790-1100kPa, and Second distillation column operating pressure is 180-350kPa；
It is preferably that pre-rectifying tower operating pressure is 40-92kPa, first rectifying column operation pressure for two: three Deethanizer design pressure of mode
Power is 650-1150kPa, and Second distillation column operating pressure is 150-220kPa.
8. the refining crude methanol process of three tower triple effect of modified according to claim 6, which is characterized in that
For mode one: the number of plates of the pre-rectifying tower is 50-58 layers, and the temperature of overhead extraction is 60-65.2 DEG C, pressure is
110-130kPa, reflux ratio 3.5-4.8, it is 75-85 DEG C that tower bottom, which produces temperature, pressure 136-160kPa；First essence
The number of plates for evaporating tower is 70-95 layers, and the temperature of overhead extraction is 115-145 DEG C, pressure 890-1050kPa, reflux ratio are
1.5-2.9, it is 145-155 DEG C that tower bottom, which produces temperature, pressure 950-1045kPa；The number of plates of the Second distillation column is 85-
95 layers, the temperature of overhead extraction is 70-105 DEG C, pressure 180-260kPa, reflux ratio 1.3-2.2, and tower bottom extraction temperature is
115-129 DEG C, pressure 220-290kPa.
For mode two: the number of plates of the pre-rectifying tower is 45-58 layers, and the temperature of overhead extraction is 42-49 DEG C, pressure is
50-60kPa, reflux ratio 2.5-4.6, it is 55-68 DEG C that tower bottom, which produces temperature, pressure 70-92kPa；The first rectifying column
The number of plates be 70-95 layers, the temperature of overhead extraction is 105-132 DEG C, pressure 690-742kPa, reflux ratio 1.4-2.9,
It is 125-145 DEG C that tower bottom, which produces temperature, pressure 720-815kPa；The number of plates of the Second distillation column is 85-95 layers, tower top
The temperature of extraction is 65-85 DEG C, pressure 150-210kPa, reflux ratio 1.4-2.9, and it is 110-120 DEG C that tower bottom, which produces temperature,
Pressure is 150-195kPa.
9. the refining crude methanol process of three tower triple effect of modified according to claim 6, which is characterized in that
For mode one: the gaseous phase materials of the pre-rectifying tower overhead extraction are successively condensed by condensation for the first time and second,
Second of condensed condensation liquid phase carries out gas-liquid separation, the isolated separation of the gentle liquid of condensation liquid phase through condensing for the first time
Liquid phase cocurrent flows back into pre-rectifying tower as phegma, and a small amount of fixed gas returns to second of condensation operation after cocurrent, through second
The isolated separation gas phase of the fixed gas phase and gas-liquid of secondary condensation carries out subsequent processing；
For mode one or mode two: the pre-rectifying tower for needing decompression operation, the gas phase of the pre-rectifying tower overhead extraction
Material is successively condensed by condensation for the first time and second, and second of condensed condensation liquid phase carries out gas-liquid separation, through first
The isolated separation liquid phase cocurrent of the gentle liquid of condensation liquid phase of secondary condensation flows back into pre-rectifying tower as phegma, after cocurrent
A small amount of fixed gas returns to second of condensation operation, after condensing the fixed gas through condensing for the second time mutually using third time with
Gas-liquid separation is carried out together through second of condensed condensation liquid phase, and the separation gas phase that gas-liquid separation obtains is by the 4th condensation
After carry out subsequent processing, and enter back into subsequent processing via vacuum pump by the 4th condensed material, the vacuum pump is simultaneously
It is associated with regulating valve；Wherein, the third time is condensed into room temperature condensation, is condensed into cryogenic condensation the 4th time.
10. the refining crude methanol process of three tower triple effect of modified according to claim 1, which is characterized in that described
The feed composition of crude carbinol can be with are as follows: methanol content 50-97w%, light component impurity 1.5-2.5w%, heavy constituent impurity 7.5-
13.5w%；Methanol content is 18-28w%, the aqueous methanol of tower bottom extraction in the gaseous phase materials of the pre-rectifying tower overhead extraction
Methanol content is 70-85w% in solution A；Methanol content is in the aqueous methanol solution B of the first rectifying column tower bottom extraction
50-75w%.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1817836A (en) * | 2006-03-10 | 2006-08-16 | 天津大学 | Double-efficient energy-saving and water-saving rectifying system and process for methanol |
| US20160108437A1 (en) * | 2013-05-28 | 2016-04-21 | Shinko Sugar Mill Co., Ltd. | Raw sugar and ethanol production method using selective fermentation |
| CN205328898U (en) * | 2016-01-14 | 2016-06-22 | 天津市天地创智科技发展有限公司 | System for triple effect evaporates rectification technology against current handles glycine mother liquor |
| CN108101748A (en) * | 2018-02-01 | 2018-06-01 | 天津市新天进科技开发有限公司 | Four tower triple effect methanol rectification energy-saving process methods and device |
| CN207537369U (en) * | 2017-10-27 | 2018-06-26 | 烟台国邦化工机械科技有限公司 | A kind of ethylene glycol multi-effect distillation system |
| CN108558603A (en) * | 2018-06-06 | 2018-09-21 | 天津奥展兴达化工技术有限公司 | A kind of refining crude methanol process of three towers triple effect |
| CN109369444A (en) * | 2018-12-07 | 2019-02-22 | 天津乐科节能科技有限公司 | Dimethylformamide is from backheat distillation system and recovery method |
| CN109761751A (en) * | 2017-11-09 | 2019-05-17 | 赵婷婷 | A kind of methanol thermal coupling multi-effect distillation method and device |
-
2019
- 2019-07-19 CN CN201910655239.5A patent/CN110327647B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1817836A (en) * | 2006-03-10 | 2006-08-16 | 天津大学 | Double-efficient energy-saving and water-saving rectifying system and process for methanol |
| US20160108437A1 (en) * | 2013-05-28 | 2016-04-21 | Shinko Sugar Mill Co., Ltd. | Raw sugar and ethanol production method using selective fermentation |
| CN205328898U (en) * | 2016-01-14 | 2016-06-22 | 天津市天地创智科技发展有限公司 | System for triple effect evaporates rectification technology against current handles glycine mother liquor |
| CN207537369U (en) * | 2017-10-27 | 2018-06-26 | 烟台国邦化工机械科技有限公司 | A kind of ethylene glycol multi-effect distillation system |
| CN109761751A (en) * | 2017-11-09 | 2019-05-17 | 赵婷婷 | A kind of methanol thermal coupling multi-effect distillation method and device |
| CN108101748A (en) * | 2018-02-01 | 2018-06-01 | 天津市新天进科技开发有限公司 | Four tower triple effect methanol rectification energy-saving process methods and device |
| CN108558603A (en) * | 2018-06-06 | 2018-09-21 | 天津奥展兴达化工技术有限公司 | A kind of refining crude methanol process of three towers triple effect |
| CN109369444A (en) * | 2018-12-07 | 2019-02-22 | 天津乐科节能科技有限公司 | Dimethylformamide is from backheat distillation system and recovery method |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113620772A (en) * | 2020-05-07 | 2021-11-09 | 北京诺维新材科技有限公司 | Cyclohexane multi-effect distillation method and device |
| CN113620839A (en) * | 2020-05-09 | 2021-11-09 | 北京诺维新材科技有限公司 | Method and device for producing acrylonitrile |
| CN112811976A (en) * | 2021-01-12 | 2021-05-18 | 江苏扬农化工集团有限公司 | Method for recovering solvent in aqueous phase of epoxy chloropropane prepared by hydrogen peroxide method |
| CN112811976B (en) * | 2021-01-12 | 2023-01-13 | 江苏扬农化工集团有限公司 | Method for recovering solvent in aqueous phase of epoxy chloropropane prepared by hydrogen peroxide method |
| CN113087597A (en) * | 2021-03-22 | 2021-07-09 | 国家能源集团宁夏煤业有限责任公司 | Method for rectifying methanol and methanol rectifying system |
| CN113979840A (en) * | 2021-11-29 | 2022-01-28 | 中国成达工程有限公司 | Three-tower differential pressure thermal coupling rectification method for separating methanol, dimethyl carbonate and phenol |
| WO2024113526A1 (en) * | 2022-11-29 | 2024-06-06 | 华陆工程科技有限责任公司 | Coupled distillation separation system and coupled distillation separation method |
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| CN115845421B (en) * | 2022-12-19 | 2023-06-30 | 滨州黄海科学技术研究院有限公司 | System and method for continuously separating perfluorinated hexanone |
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