CN109704957A - The removal methods of carbon dioxide in allyl acetate product gas - Google Patents
The removal methods of carbon dioxide in allyl acetate product gas Download PDFInfo
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- CN109704957A CN109704957A CN201711010919.9A CN201711010919A CN109704957A CN 109704957 A CN109704957 A CN 109704957A CN 201711010919 A CN201711010919 A CN 201711010919A CN 109704957 A CN109704957 A CN 109704957A
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- carbon dioxide
- allyl acetate
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Abstract
The present invention relates to a kind of removal methods of carbon dioxide in allyl acetate product gas, mainly solve the problems, such as that inert gas carbon dioxide is accumulated in existing allyl acetate production process.The present invention is refined by using by the circulation stream portions for being back to reaction zone, to remove inert gas carbon dioxide, then gas after purification is returned to the technical solution for recycling logistics and preferably solves the above problem, can be used in allyl acetate industrial production.
Description
Technical field
The present invention relates to a kind of removal methods of carbon dioxide, more particularly to dioxy in a kind of allyl acetate product gas
Change the removal methods of carbon.
Technical background
Allyl acetate is a kind of important Organic Chemicals, widely used.Allyl acetate is produced in the world today
Main method be using acetoxylation technology, propylene and oxygen to be made to pass through gas phase catalysis using propylene, oxygen and acetic acid as raw material
It reacts and generates allyl acetate.
Propylene aoxidizes production allyl acetate through catalyst in the presence of acetic acid, and reaction product includes acetic acid allyl
Ester, propylene, oxygen, acetic acid, water, carbon dioxide and possible other inert gases mixture.Reaction mixture is by separation
After isolating heavy constituent after tower cooler, obtain in light component containing propylene, oxygen, the acetic acid not reacted completely, and reaction life
At light component water, carbon dioxide and other inert gases.Light component is returned in reactor and continues after compressor boost
Reaction, therefore this burst of light component is called circulation logistics.
Inert substance in circulation logistics, if reaction system is not discharged, will continue to accumulate using carbon dioxide as representative,
The serious pressure balance and chemical balance for influencing reaction system, What is more to set off an explosion.Therefore, in the process of reaction
In, needing constantly will be except inert substance discharge system.On the other hand, the inert substance in logistics is recycled, reaction is recycled back to
In device, it is suppressed that side reaction generates, and increases the selectivity and yield of target product allyl acetate.Therefore, it is necessary to control
The amount of carbon dioxide removal can neither remove very little cumulative effect that generates and react steady, and cannot remove too many influence target
The selectivity and yield of acetic acid product allyl ester.
CN103463955A discloses a kind of technique that carbon dioxide is separated and recovered from industrial tail gas, and technical process is such as
Under: industrial tail gas enters absorb the bottom of the tower, contacts with the absorbing liquid entered at the top of absorption tower, absorbs tower reactor and obtains rich solution；Institute
Rich solution is stated by being divided into two strands through current divider after rich solution pump, first strand of rich solution is drenched from desorber top spray to be entered；Second strand of rich solution from
Desorber middle and lower part enters desorber desorption, is desorbed out the carbon dioxide with a small amount of water vapour and is gone out by desorber top row；
Enter absorption tower circulation benefit at the top of absorption tower after lean solution cooler is cooling after lean solution and first burst of rich solution heat exchange after desorption
With using absorbing liquid to contain ethyl alcohol amine solvent concentration for 20%~50%, absorb and parsing process process CIMS is complicated.
US 3970713 discloses a kind of multi-tubular reactor, and inside is 4-8 meters of length and interior diameter is the anti-of 20-50mm
Ying Guan.In typical multi-tubular reactor, catalyst is disposed in reactor tube.Heat transport fluid reactor around the outside
Pipe circulation, to remove the heat generated by reaction.Multi-tubular reactor fortune is together in the reaction with a large amount of reaction heat and extremely
The reaction of temperature-sensitive.Since relatively uniform temperature, temperature change are small from the beginning to the end for its reactor, 20 DEG C are generally less than, multitube
Reactor is commonly referred to as " isothermal reactor ".
CN202113842 discloses a kind of novel fixed bed reactors of synthesizing vinyl acetate.This reactor is certain
Heat exchanger effectiveness is improved in degree, can effectively avoid the generation of " temperature runaway " phenomenon, is also reduced the dosage of thermophore, is subtracted
The operating cost of device is lacked.But in this method, there are processing difficulties, cost of equipment is high the disadvantages of.
The existing patent of allyl acetate industry and technology are all to pay attention to the technology of preparing and reactor of catalyst at present
Improved technology, there are no in concern allyl acetate production preparation process in product gas carbon dioxide removing sulfuldioxide, this hair
It is bright targetedly to solve the problems, such as this.
Summary of the invention
It is tired that the technical problem to be solved by the present invention is to inert gas carbon dioxide in existing allyl acetate production process
Long-pending problem.A kind of removal methods of carbon dioxide in allyl acetate product gas are provided, this method is for allyl acetate
In production, have the advantages that inert gas removal efficiency is high, reaction system is stable, unit consumption is low, high income, production cost are low.
The present invention is refined by using by the circulation stream portions for being back to reactor, to remove inert gas dioxy
Change carbon, then the technical solution that gas after purification is returned to circulation logistics is preferably solved into the above problem, can be used for acetic acid alkene
In propyl ester industrial production.
To solve the above problems, The technical solution adopted by the invention is as follows: a kind of titanium dioxide in allyl acetate product gas
The reactant stream (1) of the removal methods of carbon, oxygenous, propylene and acetic acid is sent into reaction zone A, obtains crude product logistics (2), slightly
Product stream (2) is separated into product stream (3) and circulation logistics (4) in Disengagement zone (B), separates one from circulation logistics (4)
Stock as part circulation logistics (5) be sent into the lower part absorption tower C, in absorption tower it is bottom-up with from the absorption tower top C enter
Absorbing liquid (9) counter current contacting, part recycle the carbon dioxide absorbed liquid (9) in logistics (5) and absorb, and obtain rich solution (6), rich solution
(6) after the discharge of the absorption tower bottom C, it is sent into the top urea carbon dioxide stripper D；The decarbonated exhaust gas (7) of carbon dioxide removal is by inhaling
It receives tower C tower top and returns to circulation logistics (4)；Rich solution (6) be separated into urea carbon dioxide stripper D carbon dioxide (8) and
Absorbing liquid (9), carbon dioxide (8) discharge at the top of urea carbon dioxide stripper D, absorbing liquid (9) is from urea carbon dioxide stripper B
The top absorption tower A is sent into bottom.
The removal methods of carbon dioxide in the allyl acetate product gas, it is characterised in that by weight, the part
The flow for recycling logistics (5) is less than the 40% of circulation logistics (4) flow, and the preferably flow of part circulation logistics (5) is less than circulation
The 30% of logistics (4) flow.
The removal methods of carbon dioxide in the allyl acetate product gas, it is characterised in that the absorption tower C operation pressure
Power is higher than urea carbon dioxide stripper D.
The removal methods of carbon dioxide in the allyl acetate product gas, it is characterised in that the urea carbon dioxide stripper
D tower reactor is equipped with reboiler E.
The removal methods of carbon dioxide in the allyl acetate product gas, it is characterised in that the absorption tower C and dioxy
Change carbon stripper D and uses one or more of packed tower, plate column, valve tower.
The removal methods of carbon dioxide in the allyl acetate product gas, it is characterised in that the absorption tower C and dioxy
Change carbon stripper D and uses packed tower.
The removal methods of carbon dioxide in the allyl acetate product gas, it is characterised in that inhaled in the absorbing liquid (9)
Receipts agent is one of potassium carbonate, sodium carbonate or mixture.
The removal methods of carbon dioxide in the allyl acetate product gas, it is characterised in that the temperature of the absorbing liquid (9)
60 DEG C~150 DEG C of degree, preferably 80 DEG C~120 DEG C of the temperature of absorbing liquid (9), by weight, concentration of absorbing in absorbing liquid (9)
It is 10%~60%, concentration of absorbing is 15%~40% preferably in absorbing liquid (9).
In above-mentioned technical proposal, it is furthermore preferred that it is preferred that 100 DEG C~120 DEG C of the temperature of absorbing liquid (9).
In technical solution of the present invention, by material compositions such as unconverted propylene, unconverted oxygen and carbon dioxide
Circulation logistics is back in reactor, improves reactant utilization rate, is reduced production cost, is reduced the product list of allyl acetate
Consumption.
It in technical solution of the present invention, wraps carbonated by-product and is recycled back to reactor, it is suppressed that side reaction produces
It is raw, increase the selectivity and yield of target product allyl acetate.But high level inert component especially carbon dioxide follows
Loopback reactor will increase dramatically the load of reactor and the power of compressor, so that energy consumption be significantly increased.
In technical solution of the present invention, by weight, the flow that part recycles logistics (5) is less than the ratio of circulation logistics (4)
Value is less than 40%, and preferably smaller than 30%, more preferably less than 20%.If this is primarily due to not remove inert component, Jiu Huizao
At the continuous accumulation of inert component, and then the normal operation of device is influenced, or even will cause accident.If removing inert component amount
It is excessive, according to chemical reaction equilibrium, just has reactant and be converted into new inert component, can thus reduce the life of target product
Cheng Liang increases unit consumption, improves production cost, loses competitive advantage, while can also reduce the selectivity and yield of allyl acetate.
Meanwhile the flow of too small part circulation logistics (5) be less than circulation logistics (4) ratio be unfavorable for maximumlly improving yield and
Reduce energy consumption.
In technical solution of the present invention, it is preferred that the flow of part circulation logistics (5) is less than the ratio of circulation logistics (4)
It is 0.10~0.20.
In technical solution of the present invention, the flow of logistics (5) and the ratio of circulation logistics (4) can be recycled by part,
Carry out the volume content of inert component in control loop gas between 5%~40%, preferably 8%~30%, more preferable 10%~
20%, it can not only make reaction system stablize, and side reaction is few, so that the production technology tool of entire allyl acetate
Have the advantages that low unit consumption, high income, production cost are low.Using the technical solution of the invention, optimal knot can be obtained
Fruit, reaction system even running, by controlling the removal efficiency of carbon dioxide, yield can be improved 5% or more, achieve good skill
Art effect.
In another technical solution of the invention, absorbing liquid (9) and rich solution (6) carry out heat exchange, can further decrease
Energy consumption on the basis of the technical program, then reduces by 15% or more energy consumption.
Compare from the data of embodiment and comparative example as can be seen that dioxy can be made using method of the present invention
Change carbon removal efficiency height, the yield of target product increases, reduction unit consumption, to reduce production cost.Another aspect due to
The presence for recycling logistics, reduces the generation of side reaction, the yield of target product allyl acetate is made to be greatly improved.
Compare from the data of embodiment and comparative example it can also be seen that the value of " purification/circulation " needs to control certain
In range, the generation of target product allyl acetate otherwise will affect, and then influence unit consumption, energy consumption, the stability of reaction system
And the technical indicator that yield etc. is important。
Obviously, using method of the invention, with inert gas removal efficiency is high, reaction system is stable, unit consumption is low, yield
Advantage high, production cost is low, can be used in the industrial production of allyl acetate.
Using technical solution of the present invention, good technical effect is realized by selection process process, can be greatly reduced
Energy consumption.
Detailed description of the invention
Fig. 1 is the flow diagram of the method for the invention.
Fig. 2 is the flow diagram of another implementation method of the present invention.
Fig. 1, in 2,1 is reactant stream；2 be crude product logistics；3 be product stream；4 be circulation logistics；5 follow for part
Ring logistics；6 be rich solution；61 be the preceding rich solution that exchanges heat；62 be rich solution after heat exchange；7 be decarbonated exhaust gas；8 be carbon dioxide；9 are
Absorbing liquid；91 be the preceding absorbing liquid that exchanges heat；92 be absorbing liquid after heat exchange；10 be the logistics of reboiler entrance；11 export object for reboiler
Stream；A is reaction zone；B is Disengagement zone；C is absorption tower；D is urea carbon dioxide stripper；E is reboiler；F is heat exchanger.
In Fig. 1, the reactant stream (1) of oxygenous, propylene and acetic acid is sent into reaction zone A, obtains crude product logistics (2),
Crude product logistics (2) is separated into product stream (3) and circulation logistics (4) in Disengagement zone (B), separates from circulation logistics (4)
One is sent into the lower part absorption tower C as part circulation logistics (5), bottom-up in absorption tower to enter with from the absorption tower top C
Absorbing liquid (9) counter current contacting, part recycles the carbon dioxide absorbed liquid (9) in logistics (5) and absorbs, obtains rich solution (6), rich
After liquid (6) is discharged from the absorption tower bottom C, it is sent into the top urea carbon dioxide stripper D；The decarbonated exhaust gas (7) of carbon dioxide removal by
Absorption tower C tower top returns to circulation logistics (4)；Rich solution (6) is separated into carbon dioxide (8) in urea carbon dioxide stripper D
With absorbing liquid (9), carbon dioxide (8) discharge at the top of urea carbon dioxide stripper D, absorbing liquid (9) is stripped from carbon dioxide
The top absorption tower A is sent into the bottom tower B.
In Fig. 2, the reactant stream (1) of oxygenous, propylene and acetic acid is sent into reaction zone A, obtains crude product logistics (2),
Crude product logistics (2) is separated into product stream (3) and circulation logistics (4) in Disengagement zone (B), separates from circulation logistics (4)
One is sent into the lower part absorption tower C as part circulation logistics (5), bottom-up in absorption tower to enter with from the absorption tower top C
Absorbing liquid (92) counter current contacting, part recycle logistics (5) in carbon dioxide absorbed liquid (92) absorb, obtain rich solution
(61), rich solution (61) after heat exchange, obtains rich solution in heat exchanger F with absorbing liquid (91) after the discharge of the absorption tower bottom C
(62) it is sent into the top urea carbon dioxide stripper D；The decarbonated exhaust gas (7) of carbon dioxide removal returns to circulation by absorption tower C tower top
Logistics (4)；Rich solution (62) is separated into carbon dioxide (8) and absorbing liquid (91), carbon dioxide in urea carbon dioxide stripper D
Logistics (8) discharge at the top of urea carbon dioxide stripper D, absorbing liquid (91) are sent into absorption tower A from the bottom urea carbon dioxide stripper B
Top.
The present invention will be further described below by way of examples, but is not limited only to the present embodiment.
Specific embodiment
[Examples 1 to 6]
By taking 100,000 tons/year of allyl acetate device product qi exhaustion removing carbon dioxides as an example, absorption tower and carbon dioxide stripping
Tower uses packed tower, and absorbent uses potassium carbonate, and 95 DEG C of absorbent temperature, concentration of absorbing 20%, changing section recycles logistics
Flow and circulation logistics flux ratio, investigate target product allyl acetate yield situation of change, energy consumption situation of change
And absorb the changes of contents situation of carbon dioxide in tail gas.Wherein energy consumption situation of change reference standard is no carbon dioxide eliminating
The allyl acetate device of technique.
According to inventive method described in Fig. 1, result of implementation is as shown in table 1.It can be seen that part recycles the stream of logistics in table
The ratio with circulation logistics flux is measured at 0.15 or so, yield increases at most, and energy consumption reduction is than preferably designing at most
Point.According to inventive method described in Fig. 2, result of implementation on the basis of energy consumption reduction, can reduce by 15% energy in table 1 again
Consumption.
Table 1
[embodiment 7~10]
By taking 100,000 tons/year of allyl acetate device product qi exhaustion removing carbon dioxides as an example, absorption tower and carbon dioxide stripping
Packed tower, plate column, valve tower is respectively adopted in tower, and absorbent uses potassium carbonate or sodium carbonate, 95 DEG C of absorbent temperature, absorbs
Agent concentration 20%, it is 0.15 that part, which recycles the flow of logistics and the ratio of circulation logistics flux, investigates target product acetic acid allyl
Yield situation of change, energy consumption situation of change and the changes of contents situation for absorbing carbon dioxide in tail gas of ester.Wherein energy consumption becomes
Change the allyl acetate device that situation reference standard is no carbon dioxide eliminating technology.
The form of tower is little to the influential effect of absorption as can be seen from Table 2, and absorbent uses potassium carbonate or carbonic acid
Sodium uses packed tower, plate column, valve tower to embodiment knot yield and energy consumption without influence, absorption tower and urea carbon dioxide stripper
Fruit influences very little.
Table 2
[embodiment 11~15]
By taking 100,000 tons/year of allyl acetate device product qi exhaustion removing carbon dioxides as an example, absorption tower and carbon dioxide stripping
Tower uses packed tower or plate column, and absorbent uses potassium carbonate, changes absorbent temperature, and concentration of absorbing 15% partially follows
The flow of ring logistics and the ratio of circulation logistics flux are 0.15, the yield situation of change of investigation target product allyl acetate,
Energy consumption situation of change and the changes of contents situation for absorbing carbon dioxide in tail gas.Wherein energy consumption situation of change reference standard is nothing
The allyl acetate device of carbon dioxide eliminating technology.
According to inventive method described in Fig. 1, result of implementation is as shown in table 3.In table it can be seen that 100 DEG C of left sides of absorbent temperature
Youshi, yield increase at most, and it is than preferably design point that energy consumption, which is reduced at most,；The form of tower is little to the influential effect of absorption.
According to inventive method described in Fig. 2, result of implementation on the basis of energy consumption reduction, can reduce by 15% energy consumption in table 3 again.
Table 3
[embodiment 16~20]
By taking 100,000 tons/year of allyl acetate device product qi exhaustion removing carbon dioxides as an example, absorption tower and carbon dioxide stripping
Tower uses packed tower, and absorbent uses sodium carbonate, 100 DEG C of absorbent temperature, changes concentration of absorbing, part recycles the stream of logistics
The ratio of amount and circulation logistics flux is 0.15, investigates the yield situation of change of target product allyl acetate, energy consumption changes feelings
Condition and the changes of contents situation for absorbing carbon dioxide in tail gas.Wherein energy consumption situation of change reference standard is no carbon dioxide de
Except the allyl acetate device of technique.
According to inventive method described in Fig. 1, result of implementation is as shown in table 4.It can be seen that absorbent from data shown in table 4
Concentration 20% or so is than preferably design point.
As can be seen that absorbent temperature is higher in table 1~4, concentration of absorbing is higher suitable, but absorbent temperature
High and concentration height will increase material consumption and energy consumption, will increase production cost accordingly.According to inventive method described in Fig. 2, implement knot
Fruit can reduce by 15% energy consumption again on the basis of energy consumption is reduced in table 1.
Table 4
[the Comparative Examples 1 to 5]
By taking 100,000 tons/year of allyl acetate device product qi exhaustion removing carbon dioxides as an example, absorption tower and carbon dioxide stripping
Using packed tower or plate column, perhaps valve tower absorbent uses sodium carbonate or potassium acetate to tower, change absorbent temperature and
For concentration of absorbing not in the range described in the technical program, changing section recycles the flow of logistics and the ratio of circulation logistics flux
Not in the range described in the technical program, investigate the yield situation of change of target product allyl acetate, energy consumption situation of change with
And absorb the changes of contents situation of carbon dioxide in tail gas.Wherein energy consumption situation of change reference standard is no carbon dioxide eliminating work
The allyl acetate device of skill.
According to inventive method described in Fig. 1, result of implementation is as shown in table 5.
Table 5
Claims (10)
1. the removal methods of carbon dioxide, the reactant stream of oxygenous, propylene and acetic acid in a kind of allyl acetate product gas
(1) it is sent into reaction zone A, is obtained crude product logistics (2), crude product logistics (2) is separated into product stream (3) in Disengagement zone (B)
With circulation logistics (4), one is separated from circulation logistics (4) as part circulation logistics (5) and is sent into the lower part absorption tower C, is being inhaled
It receives bottom-up absorbing liquid (9) counter current contacting with from the entrance of the absorption tower top C, part in tower and recycles the dioxy in logistics (5)
Change carbon absorbed liquid (9) to absorb, obtain rich solution (6), after rich solution (6) is discharged from the absorption tower bottom C, is sent into urea carbon dioxide stripper
The top D；The decarbonated exhaust gas (7) of carbon dioxide removal returns to circulation logistics (4) by absorption tower C tower top；Rich solution (6) is in titanium dioxide
It is separated into carbon dioxide (8) and absorbing liquid (9) in carbon stripper D, carbon dioxide (8) is from urea carbon dioxide stripper D
Top discharge, absorbing liquid (9) are sent into the top absorption tower A from the bottom urea carbon dioxide stripper B.
2. according to claim 1 in allyl acetate product gas carbon dioxide removal methods, it is characterised in that with weight
The flow of meter, part circulation logistics (5) is less than the 40% of circulation logistics flux (4).
3. according to claim 2 in allyl acetate product gas carbon dioxide removal methods, it is characterised in that with weight
The flow of meter, part circulation logistics (5) is less than the 30% of circulation logistics flux (4).
4. according to claim 1 in allyl acetate product gas carbon dioxide removal methods, it is characterised in that the suction
It receives tower C operating pressure and is higher than urea carbon dioxide stripper D.
5. according to claim 1 in allyl acetate product gas carbon dioxide removal methods, it is characterised in that described two
Carbonoxide stripper D tower reactor is equipped with reboiler E.
6. according to claim 1 in allyl acetate product gas carbon dioxide removal methods, it is characterised in that the suction
It receives tower C and/or urea carbon dioxide stripper D and uses one or more of packed tower, plate column, valve tower.
7. the removal methods of carbon dioxide in allyl acetate product gas according to claim 1 or 6, it is characterised in that described
Absorption tower C and/or urea carbon dioxide stripper D uses packed tower.
8. according to claim 1 in allyl acetate product gas carbon dioxide removal methods, it is characterised in that the suction
Receiving absorbent in liquid (9) is one of potassium carbonate, sodium carbonate or mixture.
9. according to claim 1 or 8 in allyl acetate product gas carbon dioxide removal methods, it is characterised in that it is described
Temperature 60 C~150 DEG C of absorbing liquid (9), and/or by weight in absorbing liquid (9) concentration of absorbing be 10%~60%.
10. according to claim 9 in allyl acetate product gas carbon dioxide removal methods, it is characterised in that the suction
Receive 80 DEG C~120 DEG C of temperature of liquid (9), and/or by weight in absorbing liquid (9) concentration of absorbing is 15%~40%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1339423A (en) * | 2000-08-18 | 2002-03-13 | 英国石油化学品有限公司 | Purifying method for carbon dioxide containing air flow |
| WO2004078696A1 (en) * | 2003-03-07 | 2004-09-16 | Showa Denko K.K. | Production processes of lower aliphatic carboxylic acid alkenyl esters and alkenyl alcohol |
| CN102641653A (en) * | 2012-04-25 | 2012-08-22 | 中国石油化工股份有限公司 | Technology of carbon dioxide removal from reaction recycle gas of vinyl acetate monomer |
| CN102666466A (en) * | 2009-09-30 | 2012-09-12 | 莱昂德尔化学技术公司 | Process for producing allyl acetate |
| CN103463955A (en) * | 2013-09-16 | 2013-12-25 | 湖南大学 | Technology for separating and recovering carbon dioxide from industrial tail gas |
-
2017
- 2017-10-26 CN CN201711010919.9A patent/CN109704957B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1339423A (en) * | 2000-08-18 | 2002-03-13 | 英国石油化学品有限公司 | Purifying method for carbon dioxide containing air flow |
| WO2004078696A1 (en) * | 2003-03-07 | 2004-09-16 | Showa Denko K.K. | Production processes of lower aliphatic carboxylic acid alkenyl esters and alkenyl alcohol |
| CN102666466A (en) * | 2009-09-30 | 2012-09-12 | 莱昂德尔化学技术公司 | Process for producing allyl acetate |
| CN102641653A (en) * | 2012-04-25 | 2012-08-22 | 中国石油化工股份有限公司 | Technology of carbon dioxide removal from reaction recycle gas of vinyl acetate monomer |
| CN103463955A (en) * | 2013-09-16 | 2013-12-25 | 湖南大学 | Technology for separating and recovering carbon dioxide from industrial tail gas |
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