CN108558603A - A kind of refining crude methanol process of three towers triple effect - Google Patents
A kind of refining crude methanol process of three towers triple effect Download PDFInfo
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Abstract
The present invention provides a kind of refining crude methanol process of three towers triple effect, so that the refined methanol gas phase heat that compression rectification column overhead produces is met atmospheric distillation bottom of tower first and boils load again, remaining refined methanol gas phase heat boils again for pre-rectifying tower bottom of tower provides partial heat.The distribution of two parts heat enables to the heat of compression rectification column overhead gaseous phase materials to obtain maximized reasonable distribution and utilization, effectively reduces system energy consumption.
Description
Technical field
The invention belongs to chemical materials purification process and equipment technical fields, and in particular to a kind of refining crude methanol side
Method and system.
Background technology
Methanol is a kind of important basic organic chemical raw material and novel energy fuel, industrial synthesizing methanol almost all
It includes gas making, cleaning up, methanol-fueled CLC and crude carbinol rectifying to add the method for hydrogen, technical process using carbon monoxide pressurized catalysis
Etc. processes, the main task of methanol rectification be removing volatile components such as dimethyl ether, and the ethyl alcohol of difficult volatilization, higher alcohols and
Water, production meet the refined methanol of product requirement.With flourishing for coal chemical industry, the scale of methanol rectifying system is also more next
Bigger, the energy consumption for how reducing single ton of refined methanol of refining methanol device has become Business survival and improves the key of competitiveness, extensively
Big researcher is furtherd investigate as research object.
Three tower methanol rectifications (fair current double-effect rectification) technique widely used at present, i.e. crude carbinol sequence pass through pre- rectifying
Tower, compression rectification tower, atmospheric distillation tower carry out rectifying separation, are obtained respectively in the discharging of pressurization column overhead and the discharging of normal pressure column overhead
Methanol product.Separation sequence is the light component removed by pre-rectifying tower in crude carbinol, and the prognosis crude carbinol of tower reactor enters pressurization essence
Tower is evaporated, using the condensation latent heat of pressurization column overhead methanol steam as atmospheric tower boiling hot source again, realization fair current double-effect rectification, fusel
From atmospheric tower side take-off, waste water is discharged from atmospheric tower bottom of tower.This method is common refining crude methanol process, methanol rectification
Process energy consumption is about 3223.7MJ/ tons of methanol products, and energy consumption is higher, and with the expansion of refining methanol scale, gross energy disappears
Consumption also dramatically increases.
To reduce the energy consumption of methanol rectification, the prior art has a variety of trial schemes, such as adds as five tower rectifying, or
Using heat pump techniques.But five tower rectifying directly results in place, tower is invested and the other problems such as condensed water need to consume, heat pump
Rectifying also has the problem of equipment investment and power consumption.
Invention content
The purpose of the present invention is to provide a kind of refining crude methanol processes of three towers triple effect, can reduce system energy
Consumption reduces equipment investment.
The refining crude methanol process of the three tower triple effects of the present invention, the refined methanol gas phase for making compression rectification column overhead produce
Heat meets atmospheric distillation bottom of tower and boils load again first, and remaining refined methanol gas phase heat boils again for pre-rectifying tower bottom of tower provides part
Heat.The distribution of two parts heat enables to the heat of compression rectification column overhead gaseous phase materials to obtain maximized reasonable distribution
And utilization, effectively reduce system energy consumption.
Specifically, after crude carbinol enters pre-rectifying tower, light component and a small amount of gaseous methanol contain from pre-rectifying tower overhead extraction
Water methanol solution A produces from pre-rectifying tower bottom of tower and enters compression rectification tower；The refined methanol gas phase of compression rectification column overhead extraction
Material is divided into two strands：One send to atmospheric distillation tower bottom of tower and is provided for atmospheric distillation tower boils institute's calorific requirement again, another stock send to
Pre-rectifying tower bottom of tower simultaneously provides for pre-rectifying tower and boils required partial heat again；After carrying out heat exchange, two strands of refined methanol gas gas-phase objects
Material respectively becomes refined methanol lime set and merges；Refined methanol lime set after merging is divided at least two strands：One flows back as phegma
Into compression rectification tower, another strand produces as product；Compression rectification tower bottom of tower extraction aqueous methanol solution B enters atmospheric distillation
Tower；The refined methanol gaseous phase materials of atmospheric distillation tower overhead extraction are divided into two strands：One is produced as product, one forms phegma
Flow back into atmospheric distillation tower；Atmospheric distillation tower bottom of tower extracted waste water material.
The number of plates of the pre-rectifying tower is 50-60 layers, and the temperature of overhead extraction is 60-65 DEG C, pressure 110-
130kPa, reflux ratio 5.0-9.5, it is 79-83 DEG C that bottom of tower, which produces temperature, pressure 160-165kPa；The compression rectification tower
The number of plates be 70-90 layers, the temperature of overhead extraction is 120-130 DEG C, pressure 700-750kPa, reflux ratio 2.0-4.2,
It is 125-135 DEG C that bottom of tower, which produces temperature, pressure 750-800kPa；The number of plates of the atmospheric distillation tower is 80-100 layers, tower
Top extraction temperature be 70-80 DEG C, pressure 120-140kPa, reflux ratio 1.5-3.5, bottom of tower produce temperature be 110-120
DEG C, pressure 167-190kPa.
The optimal control of process conditions so that system energy consumption advanced optimizes drop in the case where ensureing refined methanol purity
It is low.
Wherein, the feed composition of the crude carbinol is：Methanol content 85-95w%, light component impurity 1.5-2.5w%, weight
Composition impurity 2.5-13.5w%；Methanol content is 60-65w% in the gaseous phase materials of the pre-rectifying tower overhead extraction, and bottom of tower is adopted
Methanol content is 70-85w% in the aqueous methanol solution A gone out；In the aqueous methanol solution A of compression rectification tower bottom of tower extraction
Methanol content is 70-75w%.The optimal control of every input and output material composition ensureing refined methanol purity, reducing energy consumption
Simultaneously, additionally it is possible to optimize purification efficiency.
Wherein, the gaseous phase materials of the pre-rectifying tower overhead extraction are condensed by condensation for the first time and for the second time laggard respectively
Row gas-liquid separation, separating liquid flow back into pre-rectifying tower as phegma, and separation gas merges with the fixed gas after time condensation
It is sent into aftertreatment systems.Condensing recovery efficiency can be improved using time condensation, reduce the turnover rate of methanol.
Wherein, the pre-rectifying tower bottom of tower has at least two reboiling devices, preferably three, wherein a reboiling device
It is coupled with wherein one progress heat of the refined methanol gaseous phase materials of compression rectification column overhead extraction.It is separately provided and refined methanol gas
Phase materials carry out the reboiling device of heat coupling, and input cost is small, and transformation is efficient, are conducive to operate and control, can be effective
The reliability of heat coupling is improved, heat flow effective rate of utilization is improved.
Wherein, the refined methanol gaseous phase materials of the compression rectification column overhead extraction become refined methanol lime set simultaneously through heat exchange
After merging, fixed gas therein merges with the gaseous phase materials of atmospheric distillation tower overhead extraction in gaseous form as third stock to be adopted
Go out.On the one hand fixed gas can be recovered further, can also avoid reentering compression rectification tower and cause energy waste and shadow
Acoustic system operation stability.
Wherein, it is divided into two strands after the refined methanol gaseous phase materials of the atmospheric distillation tower overhead extraction are condensed：One conduct
Phegma flows back into atmospheric distillation tower；Another stock-traders' know-how is further cooling to be produced as product.
Wherein, the atmospheric distillation tower middle and lower part, which also produces, fusel, and aqueous fusel is 50~80w%, the temperature of extraction
It it is 95~101 DEG C, pressure is 110~170KPa.The design of fusel extraction circuit advantageously reduces atmospheric distillation tower load, improves
Refining methanol efficiency further decreases energy consumption, and the fusel after recycling can also obtain resource utilization utilization after further treatment.
Compared with prior art, the present invention has the advantage that：The easily controllable implementation of process, equipment investment is small, can
Strong operability can effectively reduce refining methanol specific energy consumption, without occupying additional place, it is easy to accomplish to the fast of existing engineering
Speed transformation.
Description of the drawings
The attached drawing for constituting the part of the present invention is used to provide further understanding of the present invention, schematic reality of the invention
Example and its explanation are applied for explaining the present invention, is not constituted improper limitations of the present invention.In the accompanying drawings：
Fig. 1 is the process flow chart of the present invention.Wherein thick blue line is liquid phase process logistics, and fine powder colo(u)r streak is gas phase process
Logistics.
Specific implementation mode
In order to better understand the present invention, 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, following example has carried out the explanation of many process details, is not intended to cause improper restriction to the present invention.
As shown in Figure 1, crude carbinol (material R1) enters through the first preheater M4 preheatings in pre-rectifying tower M1, feeding temperature 60
DEG C, 52 floor heights of setting imitate DVST column plates in tower.Light component and a small part gaseous form methanol in crude carbinol are from pre-rectifying tower
M1 overhead extractions, methanol content is about 63% in the gaseous phase materials of overhead extraction, and the temperature of overhead extraction is 64.7 DEG C, and pressure is
The gaseous phase materials of 129KPa, overhead extraction pass through the first condenser M5 respectively and the second condenser M6 carries out time condensation, material
40 DEG C are cooled to, the fixed gas after time condensation is sent into follow-up flare system, and the condensate liquid after time condensation is sent into gas-liquid separation
Device M7 carries out further gas-liquid separation, and the separating liquid after gas-liquid separation enters the top the of pre-rectifying tower M1 through the first return tank M8
52 layers of column plate flow back, reflux ratio 5.5,40 DEG C of phegma temperature, after the separation gas after gas-liquid separation and time condensation
Fixed gas merge and be sent into follow-up flare system.Condensate liquid in first condenser M5 is directly entered the first return tank M8, and first
Fixed gas in return tank M8 mutually flows back into the second condenser M6 and continues to condense.
The bottoms the pre-rectifying tower M1 are parallel at least two reboilers, and this example is three, respectively reboiler M9, is boiled again
Device M10 and reboiler M11.Reboiler M10 and reboiler M11 carries out heat supply by external steam pipeline respectively.Wherein one again
Boil device M11 sides and be equipped with surge tank M12, the gaseous phase materials of self-pressurization rectifying column M2 overhead extractions enter surge tank M12, then with
Reboiler M11 carries out thermal coupling (heat exchange) cooling and forms lime set, and lime set returns to the second return tank M16 of compression rectification tower M2.
The bottoms of tower the pre-rectifying tower M1 produce aqueous methanol solution A (material R2), and wherein methanol content is about 83.6%, tower
The temperature of bottom extraction is 80.4 DEG C, pressure 1.6kg/cm2.Aqueous methanol solution A enters after the second preheater M13 preheatings
On the middle and lower part column plate of compression rectification tower M2,125 DEG C of feeding temperature.Second preheater M13 is carried out by external steam pipeline
Heat supply.85 floor heights of setting imitate DVST column plates in compression rectification tower M2 towers.The gaseous phase materials of overhead extraction are refined methanol, methanol content
It is 99.991%, the temperature of overhead extraction is 122.6 DEG C, pressure 7.0kg/cm2.The refined methanol gaseous phase materials of overhead extraction point
It is two strands：One (material R4) is preferentially entered in the reboiler M19 of the bottoms of tower atmospheric distillation tower M3, is provided and be disclosure satisfy that reboiler
Institute's calorific requirement of M19, makes the process of boiling again of the bottoms of tower atmospheric distillation tower M3 that need not be re-introduced into external heat source, is condensed after heat exchange
The refined methanol lime set got off enters in the second return tank M16 of compression rectification tower M2；Another stock (material R5) as previously mentioned, into
In the reboiler M11 of the bottoms pre-rectifying tower M1, institute's calorific requirement is provided for reboiler M11, the bottoms of tower pre-rectifying tower M1 is reduced and boiled again
The steam total flow of Cheng Suoxu, the refined methanol lime set condensed out after heat exchange also enter in the second return tank M16.Second
Refined methanol lime set material in return tank M16 is also classified into two strands or three strands：One enters the 85th layer of the top of compression rectification tower M2
Column plate flows back, reflux ratio 2.2,122.6 DEG C of phegma temperature；Second strand cold through the first cooler M17 and second successively
But device M18 enters product storage tank after carrying out secondary cooling；Third stock in gaseous form with atmospheric distillation tower M3 overhead extractions
Gaseous phase materials are combined into third condenser M20, and third stock is to contain when in the refined methanol lime set being back in the second return tank M16
It is formed when having certain fixed gas, not generating fixed gas under some conditions, then this strand of material is not present.
The bottoms compression rectification tower M2 are parallel with an at least reboiler, and this example is two, respectively reboiler M14 and
Reboiler M15, the two carry out heat supply by external steam pipeline respectively.
The bottoms of tower the compression rectification tower M2 extraction aqueous methanol solution B (material R3), wherein methanol content is about 70.3%,
The temperature of bottom of tower extraction is 132.7 DEG C, pressure 7.6kg/cm2.Aqueous methanol solution B enters the middle and lower part of atmospheric distillation tower M3
On column plate, 125 DEG C of feeding temperature.90 floor heights of setting imitate DVST column plates in atmospheric distillation tower M3 towers.The gas gas-phase objects of overhead extraction
Material is refined methanol (material R6), and the temperature of methanol content 99.994%, overhead extraction is 72.3 DEG C, pressure 1.4kg/cm2。
The refined methanol gaseous phase materials of overhead extraction, which enter through third condenser M20 in third return tank M21, carries out condensation cooling, and condensation is cold
But the material after is divided into two strands：One flows back into the 90th layer of the top column plate of atmospheric distillation tower M3, reflux ratio 1.7,
72.3 DEG C of phegma temperature；Enter product storage tank after another stock-traders' know-how third cooler M22 coolings.
Atmospheric distillation tower M3 bottom of tower extracted waste water materials (material R7), wherein aqueous is 99.8%, bottom of tower extraction
Temperature is 114.1 DEG C, pressure 1.7kg/cm2.After the 4th cooler M25 cooling, be transported to follow-up waste disposal system into
Row processing.
The middle and lower parts the atmospheric distillation tower M3 are additionally provided with fusel (material R8) extraction mouth, main to be enriched with the fusels such as ethyl alcohol,
In it is aqueous be 70.0%, the temperature of extraction is 40 DEG C, pressure 1.7kg/cm2.The fusel of extraction is successively through the 5th cooler M23
It is sent into fusel tank field with the second surge tank M24.
In above-mentioned technical process, the composition of correlative is as shown in table 1.
1 material of table forms unit w%
| Stock number | R1 | R2 | R3 | R4 | R5 | R6 | R7 | R8 |
| H2 | 0.0011 | 0 | 0 | 0 | 0 | 0 | 0 | 0 |
| CO | 0.0028 | 0 | 0 | 0 | 0 | 0 | 0 | 0 |
| CO2 | 2.1701 | 0 | 0 | 0 | 0 | 0 | 0 | 0 |
| Methane | 0.0139 | 0 | 0 | 0 | 0 | 0 | 0 | 0 |
| Ethane | 0.005 | 0 | 0 | 0 | 0 | 0 | 0 | 0 |
| N2 | 0.0105 | 0 | 0 | 0 | 0 | 0 | 0 | 0 |
| Methanol | 87.9496 | 83.58539 | 70.36215 | 99.99084 | 99.99084 | 99.99411 | 0.172795 | 17.55007 |
| Ethyl alcohol | 0.15 | 0.14285 | 0.254428 | 0.004482 | 0.004482 | 0.005685 | 0.021437 | 6.825496 |
| Methyl ether | 0.04 | 0 | 0 | 0 | 0 | 0 | 0 | 0 |
| Pentane | 0.00667 | 0 | 0 | 0 | 0 | 0 | 0 | 0 |
| Isopentane | 0.00667 | 0 | 0 | 0 | 0 | 0 | 0 | 0 |
| Octane | 0.00667 | 0 | 0 | 0 | 0 | 0 | 0 | 0 |
| Isobutanol | 0.02925 | 0.027854 | 0.050307 | 6.91E-22 | 6.91E-22 | 1.96E-23 | 0.002096 | 1.398562 |
| Propyl alcohol | 0.02925 | 0.027854 | 0.050307 | 7.60E-17 | 7.60E-17 | 5.37E-18 | 0.002151 | 1.398149 |
| N-butanol | 0.02925 | 0.027854 | 0.050307 | 8.80E-28 | 8.80E-28 | 0 | 0.000555 | 1.410152 |
| Amylalcohol | 0.02925 | 0.027854 | 0.050307 | 0 | 0 | 0 | 0.000185 | 1.412927 |
| Ethyl acetate | 0.028 | 8.12E-10 | 1.10E-13 | 1.63E-09 | 1.63E-09 | 1.58E-13 | 1.26E-26 | 9.85E-25 |
| Acetone | 0.007 | 0.002282 | 0.00014 | 0.004494 | 0.004494 | 0.0002 | 2.80E-16 | 1.12E-12 |
| Water | 9.485 | 16.15806 | 29.18206 | 0.000188 | 0.000188 | 1.77E-07 | 99.80078 | 70.00464 |
In above-mentioned technical process, enable the refined methanol gas phase heat reasonable distribution of compression rectification tower M2 overhead extractions,
Meet the bottoms of tower atmospheric distillation tower M3 first and boil load again, after-heat boils again for the bottoms of tower pre-rectifying tower M1 provides partial heat, subtracts
Small pre-rectifying tower M1 boils bottom of tower required external steam heat again so that the total energy consumption of system is effectively reduced, and is reduced and set
Standby investment.The heat of wherein compression rectification tower M2 and atmospheric distillation tower M3 is coupled as two effect rectifying, compression rectification tower M2 and pre- essence
The heat for evaporating tower M1 is coupled as three-effect rectification.
Using the above scheme, certain 600,000 tons/year of refining crude methanol producer is transformed, the charging of 96.72t/h crude carbinols.
Refined methanol purity is 99.9% before transformation, 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 99.9%, system energy consumption 37.8MKcal/h, methanol after transformation
Produced quantity is 84.5t/h, and the steam consumption of single ton of refined methanol is 0.89.Traditional handicraft is intersected at, system energy consumption reduces
35%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (9)
1. a kind of refining crude methanol process of three towers triple effect keeps the refined methanol gas phase heat that compression rectification column overhead produces first
First meet atmospheric distillation bottom of tower and boil load again, remaining refined methanol gas phase heat boils again for pre-rectifying tower bottom of tower provides partial heat.
2. the refining crude methanol process of three towers triple effect according to claim 1, which is characterized in that crude carbinol enters pre-
After rectifying column, from pre-rectifying tower overhead extraction, aqueous methanol solution A is adopted from pre-rectifying tower bottom of tower for light component and a small amount of gaseous methanol
Go out and enters compression rectification tower；The refined methanol gaseous phase materials of compression rectification column overhead extraction are divided into two strands：One send to normal pressure essence
It evaporates tower bottom of tower and is provided for atmospheric distillation tower and boil institute's calorific requirement again, another stock send to pre-rectifying tower bottom of tower and provided for pre-rectifying tower
Required partial heat is boiled again；After carrying out heat exchange, two strands of refined methanol gaseous phase materials respectively become refined methanol lime set and merge；It closes
Refined methanol lime set after and is divided at least two strands：One flows back into compression rectification tower as phegma, and another strand is used as product
Extraction；Compression rectification tower bottom of tower extraction aqueous methanol solution B enters atmospheric distillation tower；The refined methanol of atmospheric distillation tower overhead extraction
Gaseous phase materials are divided into two strands：One is produced as product, one forms phegma and flows back into atmospheric distillation tower；Atmospheric distillation tower
Bottom of tower extracted waste water material.
3. the refining crude methanol process of three towers triple effect according to claim 1, which is characterized in that the pre-rectifying tower
The number of plates be 50-60 layers, the temperature of overhead extraction is 60-65 DEG C, pressure 110-130kPa, reflux ratio 5.0-9.5, tower
It is 79-83 DEG C that bottom, which produces temperature, pressure 160-165kPa；The number of plates of the compression rectification tower is 70-90 layers, overhead extraction
Temperature be 120-130 DEG C, pressure 700-750kPa, reflux ratio 2.0-4.2, bottom of tower produce temperature be 125-135 DEG C, pressure
Power is 750-800kPa；The number of plates of the atmospheric distillation tower is 80-100 layers, and the temperature of overhead extraction is 70-80 DEG C, pressure
For 120-140kPa, reflux ratio 1.5-3.5, it is 110-120 DEG C that bottom of tower, which produces temperature, pressure 167-190kPa.
4. the refining crude methanol process of three towers triple effect according to claim 1, which is characterized in that the crude carbinol
Feed composition is：Methanol content 85-95w%, light component impurity 1.5-2.5w%, heavy constituent impurity 2.5-13.5w%；It is described pre-
Rectifying column tower top extraction gaseous phase materials in methanol content be 60-65w%, bottom of tower extraction aqueous methanol solution A in methanol contain
Amount is 70-85w%；Methanol content is 70-75w% in the aqueous methanol solution A of compression rectification tower bottom of tower extraction.
5. the refining crude methanol process of three towers triple effect according to claim 1, which is characterized in that the pre-rectifying tower
The gaseous phase materials of overhead extraction carry out gas-liquid separation after first time condensation and second condense respectively, and separating liquid is as reflux
Liquid flows back into pre-rectifying tower, and separation gas merges with the fixed gas after time condensation is sent into aftertreatment systems.
6. the refining crude methanol process of three towers triple effect according to claim 1, which is characterized in that the pre-rectifying tower
Bottom of tower has at least two reboiling devices, preferably three, wherein the essence of a reboiling device and the extraction of compression rectification column overhead
Wherein one progress heat coupling of methanol vapor phase material.
7. the refining crude methanol process of three towers triple effect according to claim 1, which is characterized in that the compression rectification
The refined methanol gaseous phase materials of column overhead extraction are after heat exchange becomes refined methanol lime set and merges, and fixed gas therein is as the
Three strands merge extraction with the gaseous phase materials of atmospheric distillation tower overhead extraction in gaseous form.
8. the refining crude methanol process of three towers triple effect according to claim 1, which is characterized in that the atmospheric distillation
Column overhead extraction refined methanol gaseous phase materials it is condensed after be divided into two strands：One flows back into atmospheric distillation tower as phegma；
Another stock-traders' know-how is further cooling to be produced as product.
9. the refining crude methanol process of three towers triple effect according to claim 1, which is characterized in that the atmospheric distillation
Tower middle and lower part, which also produces, fusel, and it is 50~80w% that fusel is aqueous, and the temperature of extraction is 95~101 DEG C, and pressure is 110~
170KPa。
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| CN110256202A (en) * | 2019-07-08 | 2019-09-20 | 张兵 | A kind of refining crude methanol process of four towers quadruple effect |
| CN110327647A (en) * | 2019-07-19 | 2019-10-15 | 张兵 | A kind of refining crude methanol process of three tower triple effect of modified |
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| 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 |
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