CN203999449U - The methyl nitrite reactive distillation column of synthetic gas preparing ethylene glycol - Google Patents
The methyl nitrite reactive distillation column of synthetic gas preparing ethylene glycol Download PDFInfo
- Publication number
- CN203999449U CN203999449U CN201420345468.XU CN201420345468U CN203999449U CN 203999449 U CN203999449 U CN 203999449U CN 201420345468 U CN201420345468 U CN 201420345468U CN 203999449 U CN203999449 U CN 203999449U
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- tower
- rectifying
- section
- distillation column
- ethylene glycol
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Abstract
The utility model discloses the methyl nitrite reactive distillation column of synthetic gas preparing ethylene glycol, it comprises rectifying tower, described rectifying tower is made up of the rectifying section on top and the profit reduction and reserving section of bottom, described rectifying section height is 2.3-2.5 times of profit reduction and reserving section height, rectifying section tower diameter is 1.8-2.2 times of profit reduction and reserving section tower diameter, described rectifying section inside is provided with structured packing, and profit reduction and reserving intersegmental part district is provided with float valve filler.Reactive distillation column of the present utility model, can produce the highest most economical methyl nitrite intermediates of yield for synthetic gas preparing ethylene glycol, and operational path is more optimized, and reduces the production cost of synthetic gas preparing ethylene glycol.
Description
Technical field
The utility model relates to the methyl nitrite reactive distillation column of synthetic gas preparing ethylene glycol.
Background technology
Ethylene glycol is a kind of important Elementary Chemical Industry organic raw material, mainly for the production of polyester (can further produce polyster fibre, beverage bottle, film etc.), frostproofer etc.Polyester is the main consumer field of China's ethylene glycol, and its consumption accounts for 94% of gross domestic consumption amount at present, and the polyester carbon fiber strength of its production is high, corrosion resistant, is universally acknowledged without the high-new engineering materials of harm.
Traditional ethylene glycol production method is to walk petrochemical complex route, obtains ethene by refining of petroleum, then oxidation of ethylene is generated to oxyethane, by ethylene oxide hydration generating glycol.Along with the day by day shortage of world petroleum resource, opening up new operational path has become the task of top priority.The energy structure of considering China is that coal heavy wool is few, the route of development taking producing synthesis gas from coal as waste ethylene glycol, for the reasonable utilization of China's energy, reduce dependence to oil, the deficiency that solves ethene supply all has extremely profound meaning justice." coal-ethylene glycol ", especially domestic common concern Coal Chemical Industry novel technique in the world today.Facts have proved, this route is technical feasible; Coal-ethylene glycol technological line is long, and full scale plant is progressively in maturation, and its industrial prospect is good.
With coal processing synthetic gas CO+H
2esterification unit in reaction for preparing glycol is the O containing NO circulation technology gas, out-of-bounds sending here that carbonylation unit is come
2, NO
2mixed gas, under temperature (100 DEG C), pressure (0.3MPa) operating mode, send into MN reactive distillation column, carry out esterification with the methyl alcohol acidic aqueous solution of tower top spray, generate methyl nitrite (MN), and carry out gas-liquid separation, the gas that overhead extraction contains methyl nitrite (MN), send carbonylation unit as raw material.Under this reaction normal pressure, catalyst-free, temperature carry out under the condition of 30-80 DEG C: 2NO+2CH
3oH+1/2O
2→ 2CH
3oNO+H
2o.
Summary of the invention
The purpose of this utility model is to provide one can either carry out esterification can carry out again rectifying, obtains the methyl nitrite reactive distillation column of the synthetic gas preparing ethylene glycol of higher yields methyl nitrite product simultaneously.
The methyl nitrite reactive distillation column of synthetic gas preparing ethylene glycol of the present utility model, comprise rectifying tower, described rectifying tower comprises the rectifying section on top and the profit reduction and reserving section of bottom, described rectifying section height is 2-3 times of profit reduction and reserving section height, rectifying section tower diameter is 2-4 times of profit reduction and reserving section tower diameter, described rectifying section inside is provided with structured packing, and profit reduction and reserving intersegmental part district is provided with float valve filler.
Two-way bent ripple filler is selected in described structured packing, and described float valve filler is selected guiding ladder-shaped float valve.
The tower top outlet of described rectifying tower is connected with trim the top of column device.
Described trim the top of column device comprises rectifying tower condenser and rectifying tower return tank, the import of described rectifying tower condenser connects tower top outlet by pipeline, the import of described rectifying tower return tank is connected with the outlet of rectifying tower condenser by pipeline, an outlet of described rectifying tower return tank is connected to the tower top of rectifying tower by reflux pump, another outlet of rectifying tower return tank is connected to gas phase and goes to carbonylation unit.
The tower bottom outlet of described profit reduction and reserving section is connected with reflux at the bottom of tower.
At the bottom of described tower, reflux comprises the rectifying tower water cooler being connected with tower bottom outlet, and the outlet of described rectifying tower water cooler is connected to the position, middle and lower part of rectifying section by pipeline, and described tower bottom outlet is also connected to methanol distillation column by pipeline.
Install material benzenemethanol opening for feed in the upper position of described rectifying section, be provided with the import of esterification circulation gas in described profit reduction and reserving section with the connection section of rectifying section.
The filler of the utility model rectifying section adopts two-way bent ripple filler to have another name called CHAOPAK filler.Its constructional feature is: two-directional corrugations, bending channel, be tiltedly staggered, half-twist install.Corrugated cardboard sheet has two kinds of embossing, horizontal wrinkle or bidirectional point ripple.Inverse wavelet line punching shape parallelogram, rectangle or Long Circle; Model has 250Y.Two-way bent ripple filler, the Pressure Drop of every meter of filler is all lower than unidirectional oblique wave, two-way oblique-wave and unidirectional bent ripple filler, and flux ratio three is large, is more low pressure drop, more high-throughout structured packing of one.Its pressure drop is lower based on 2 points: the one, and adjacent two dish filler wavy channels have become 135 ° of bends by 135 ° of wedge angles of unidirectional oblique wave filler; The 2nd, except the main ripple air flue of unidirectional oblique wave filler oblique mistake, also have and main airway gas-distributing channel that interlock, that formed by reverse ripple.Main airway and gas-distributing channel have formed air flue network obliquely upward, and therefore the unidirectional bent ripple filler of flux ratio still can improve more than 5%.
The full tower design of former rectifying tower is all Stainless Steel Cloth structured packing, because esterification is to complete in profit reduction and reserving section, float valve filler more easily reacts, esterification is a gas-phase reaction, the gas-to-liquid contact area of evidence on valve tray is larger, heat-transfer effect is better, more easily sends out reaction, and esterification is a moment reaction.Original rectifying tower (profit reduction and reserving section) is all structured packings, is unfavorable for esterification; Original rectifying tower rectifying section is the same with profit reduction and reserving section tower diameter, is unfavorable for esterification, has not only improved esterification effect and also reduced rectifying tower production cost after improvement; Original condenser setting is interior cool condenser, in tower top, be total reflux exactly, do not consider esterification problem completely, and that the utility model condenser is set to is outer cold, calculate reflux ratio according to the maximization of esterification, instead of calculate reflux ratio according to rectifying tower principle, because this tower Main Function is esterification, be secondly rectifying tower effect; Former rectifying tower does not have the circulation of liquid at the bottom of tower, and the utility model has been set up refluxing again of tower bottoms, and a part of tower bottoms goes methanol distillation column to reclaim methyl alcohol, and a part of tower bottoms is returned rectifying section, thereby better saves methyl alcohol, reduces methanol distillation column consumption; The utility model is in order to complete better esterification, and design has reduced opening for feed.
Profit reduction and reserving section filler of the present utility model is selected guiding ladder-shaped float valve, and guiding ladder-shaped float valve designs the high-performance valve tray of research and development on the basis of drawing the column plate experiences such as domestic and international application rectangular valve, solid tongue and Linde sieve tray.Valve block has absorbed the feature of V-type screen, changes rectangle valve block into trapezoidal valve block, makes the liquid effect that pushes away of air-flow obtain reinforcement, and the front of valve body increases a perforate, in real performance guide effect, has strengthened the liquid effect that pushes away of valve body.Structurally, can the fluctuate float valve structure of adjustments of gas circulation area of employing, has overcome the little shortcoming of V-type screen turndown ratio.Experimental study and practical application show, adopt ejection-type guiding ladder-shaped float valve to make the performance of column plate obtain larger improvement.
Rectifying section and profit reduction and reserving section have adopted different filler modes, it is advantageous that: be 1. difficult for stuck and come off, unsymmetrical structure is difficult for wrongly installed direction, simple installation; 2. the liquid of uniqueness stream promotion mechanism reduces gradient of liquid level and backmixing of liquid phase degree on column plate greatly; 3. dry-plate pressure drop and total anode drop reduce greatly; 4. leakage lower limit reduces greatly; 5. mist entrainment is little; 6. plate supernatant layer height reduces; 7. performance of anti-blockage strengthens 8. mass-transfer performances raisings.9. turndown ratio and stability improve.
The utility model methyl nitrite reactive distillation column is the production of methyl nitrite, is the important the first step of synthesizing glycol; The reaction of the utility model methyl nitrite need to not complete in specific reactor, in this rectifying tower, can complete, it is again rectifying tower that this rectifying tower is not only reaction tower, and this reaction is easy to carry out, and does not need catalyzer, temperature of reaction between 30-80 DEG C, normal pressure.
From the mixed gas of carbonylation unit, by compressor, mixed gas is delivered to esterification unit, enter reactive distillation column of the present utility model bottom.In the i.e. section of profit reduction and reserving of conversion zone of reactive distillation column,, there is esterification in the methanol solution counter current contact of circulation gas and top spray, generates methyl nitrite and water, is attended by side reaction simultaneously and generates nitric acid.Top of tower is provided with water cooler, and tower top outlet gas is cooled to 5 DEG C, isolates after liquid phase backflow wherein, and gas phase is sent to carbonylation unit.Tower reactor is the methanol aqueous solution that contains a small amount of nitric acid, and after the supercharging of reactive distillation column tower reactor pump, part is circulated to rectifying tower middle part, and part is delivered to methanol distillation column.
Also can there is esterification in former rectifying tower, but esterification is not the object of final rectifying tower, also in intrinsic rectifying tower, can not well carry out esterification, and the utility model is to design taking esterification as object, original design reaction is a reactive liquid solution:
CH
3oH (l)+HONO (l) → CH
3oNO (l) (methyl nitrite)+H
2o (l)
And reaction after the utility model improves is gas liquid reaction: because gas liquid reaction better effects if.
CH
3OH (l) + N
2O
3(g) → CH
3ONO (g) + H
2O (l)
Reactive distillation column of the present utility model, can produce the highest most economical methyl nitrite intermediates of yield for synthetic gas preparing ethylene glycol, and operational path is more optimized, and reduces the production cost of synthetic gas preparing ethylene glycol.
Brief description of the drawings
Fig. 1 is structural representation of the present utility model.
In figure: 1, rectifying tower; 11 rectifying sections; 12, profit reduction and reserving section; 2, rectifying tower reboiler; 3, rectifying tower water cooler; 4, rectifying tower condenser; 5, rectifying tower return tank; 6, reflux pump; 7, tower reactor recycle pump.
Embodiment
As shown in Figure 1, the methyl nitrite reactive distillation column of synthetic gas preparing ethylene glycol of the present utility model, comprise rectifying tower 1, rectifying tower 1 comprises the rectifying section 11 on top and the profit reduction and reserving section 12 of bottom, the connection section of rectifying section 11 and profit reduction and reserving section 12 is transition section, rectifying section 11 is highly for retaining a percentage of the total profits for the enterprise's own use section 12 2-3 highly doubly, rectifying section 11 tower diameters are 2-4 times of profit reduction and reserving section 12 tower diameters, described rectifying section 11 inside are provided with structured packing--two-way bent ripple filler, and profit reduction and reserving section 12 inner area are provided with float valve filler--guiding ladder-shaped float valve; The tower top outlet of rectifying tower 1 is connected with trim the top of column device; Trim the top of column device comprises rectifying tower condenser 4 and rectifying tower return tank 5, the import of rectifying tower condenser 4 connects tower top outlet by pipeline, the import of rectifying tower return tank 5 is connected with the outlet of rectifying tower condenser 4 by pipeline, an outlet of rectifying tower return tank 5 is connected to the tower top of rectifying tower 1 by reflux pump, another outlet of rectifying tower return tank 5 is connected to gas phase and goes to carbonylation unit; The tower bottom outlet of profit reduction and reserving section 12 is connected with reflux at the bottom of tower; At the bottom of tower, reflux comprises the rectifying tower water cooler 3 being connected with tower bottom outlet, and the outlet of rectifying tower water cooler 3 is connected to the position, middle and lower part of rectifying section 11 by pipeline, and tower bottom outlet is also connected to methanol distillation column by pipeline; Installed material benzenemethanol opening for feed in the upper position of described rectifying section 11, material benzenemethanol can be extraneous fresh methanol or from methanol distillation column, is provided with the import of esterification circulation gas in described profit reduction and reserving section 12 with the connection section of rectifying section 11.
As shown in Figure 1, rectifying tower height of the present utility model can be designed as 36300mm, the high 10450mm of profit reduction and reserving section, the high 25300mm of rectifying section (11), rectifying section (11) tower diameter 4200mm, profit reduction and reserving section (12) tower diameter 1200mm, manufacturing condition: pressure 0.3-0.4MPaG, tower reactor temperature 80-100 DEG C, tower top outlet temperature: 5 DEG C, mixing gas component: N
2, CO, NO, MN(methyl nitrite), CH3OH.The reaction principle of reactive distillation column:
Total reaction: 2NO+2CH
3oH+1/2O
2→ 2CH
3oNO+H
2o
Reaction process: 2NO+O
2=2NO
2nO
2+ NO=N
2o
32CH
3oH+N
2o
3=2 CH
3oNO(methyl nitrite)+H
2o CH
3oH+N
2o
3=CH
3oNO+HONO CH
3oH+HONO=CH
3oNO+H
2o
The utility model methyl nitrite reactive distillation column is the production of methyl nitrite, is the important the first step of synthesizing glycol; The reaction of the utility model methyl nitrite need to not complete in specific reactor, in this rectifying tower, can complete, it is again rectifying tower that this rectifying tower is not only reaction tower, and this reaction is easy to carry out, and does not need catalyzer, temperature of reaction between 80-100 DEG C, normal pressure.
By compressor, esterification recycle gas is delivered to esterification unit, enter reactive distillation column of the present utility model bottom.In the i.e. section of profit reduction and reserving of conversion zone of reactive distillation column,, there is esterification in the methanol solution counter current contact of circulation gas and top spray, generates methyl nitrite and water, is attended by side reaction simultaneously and generates nitric acid.Top of tower is provided with water cooler, and tower top outlet gas is cooled to 5 DEG C, isolates after liquid phase backflow wherein, and gas phase is sent to carbonylation unit.Tower reactor is the methanol aqueous solution that contains a small amount of nitric acid, after the supercharging of reactive distillation column tower reactor pump, part is circulated to rectifying tower middle part, part is delivered to methanol distillation column, obtain tower top component and (comprise nitrogen, carbon monoxide, nitrogen protoxide, methyl nitrite, methyl alcohol) in methyl nitrite molar fraction at 10-13%, and adopt in prior art gained tower top component methyl nitrite molar fraction generally at 5-7%, it is reactive distillation column of the present utility model, can produce the highest most economical methyl nitrite intermediates of yield for synthetic gas preparing ethylene glycol, and operational path is more optimized, reduce the production cost of synthetic gas preparing ethylene glycol.
Claims (7)
1. the methyl nitrite reactive distillation column of synthetic gas preparing ethylene glycol, comprise rectifying tower (1), it is characterized in that, described rectifying tower (1) comprises the rectifying section (11) on top and the profit reduction and reserving section (12) of bottom, described rectifying section (11) is highly profit reduction and reserving sections (12) 2-3 highly times, doubly, described rectifying section (11) inside is provided with structured packing to the 2-4 that rectifying section (11) tower diameter is profit reduction and reserving section (12) tower diameter, and profit reduction and reserving section (12) inner area is provided with float valve filler.
2. the methyl nitrite reactive distillation column of synthetic gas preparing ethylene glycol as claimed in claim 1, is characterized in that, two-way bent ripple filler is selected in described structured packing, and described float valve filler is selected guiding ladder-shaped float valve.
3. the methyl nitrite reactive distillation column of synthetic gas preparing ethylene glycol as claimed in claim 1, is characterized in that, the tower top outlet of described rectifying tower (1) is connected with trim the top of column device.
4. the methyl nitrite reactive distillation column of synthetic gas preparing ethylene glycol as claimed in claim 3, it is characterized in that, described trim the top of column device comprises rectifying tower condenser (4) and rectifying tower return tank (5), the import of described rectifying tower condenser (4) connects tower top outlet by pipeline, the import of described rectifying tower return tank (5) is connected with the outlet of rectifying tower condenser (4) by pipeline, an outlet of described rectifying tower return tank (5) is connected to the tower top of rectifying tower (1) by reflux pump, another outlet of rectifying tower return tank (5) is connected to gas phase and goes to carbonylation unit.
5. the methyl nitrite reactive distillation column of synthetic gas preparing ethylene glycol as claimed in claim 1, is characterized in that, the tower bottom outlet of described profit reduction and reserving sections (12) is connected with reflux at the bottom of tower.
6. the methyl nitrite reactive distillation column of synthetic gas preparing ethylene glycol as claimed in claim 5, it is characterized in that, at the bottom of described tower, reflux comprises the rectifying tower water cooler (3) being connected with tower bottom outlet, the outlet of described rectifying tower water cooler (3) is connected to the position, middle and lower part of rectifying section (11) by pipeline, described tower bottom outlet is also connected to methanol distillation column by pipeline.
7. the methyl nitrite reactive distillation column of synthetic gas preparing ethylene glycol as claimed in claim 1, it is characterized in that, upper position at described rectifying section (11) has installed material benzenemethanol opening for feed, is provided with the import of esterification circulation gas at described profit reduction and reserving sections (12) and the connection section of rectifying section (11).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420345468.XU CN203999449U (en) | 2014-06-26 | 2014-06-26 | The methyl nitrite reactive distillation column of synthetic gas preparing ethylene glycol |
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|---|---|---|---|
| CN201420345468.XU CN203999449U (en) | 2014-06-26 | 2014-06-26 | The methyl nitrite reactive distillation column of synthetic gas preparing ethylene glycol |
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|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105688608A (en) * | 2016-02-19 | 2016-06-22 | 宁波金远东石化工程技术有限公司 | Method for removing acid gas and moisture in outlet gas of esterification part and device of method |
-
2014
- 2014-06-26 CN CN201420345468.XU patent/CN203999449U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105688608A (en) * | 2016-02-19 | 2016-06-22 | 宁波金远东石化工程技术有限公司 | Method for removing acid gas and moisture in outlet gas of esterification part and device of method |
| CN105688608B (en) * | 2016-02-19 | 2018-04-10 | 宁波金远东石化工程技术有限公司 | Purify the method and its device of sour gas and moisture in esterification portion exit gas |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20141210 Termination date: 20180626 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |