CN110343044A - Synthesizing vinyl acetate ester reaction solution separating technology - Google Patents
Synthesizing vinyl acetate ester reaction solution separating technology Download PDFInfo
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- CN110343044A CN110343044A CN201910670036.3A CN201910670036A CN110343044A CN 110343044 A CN110343044 A CN 110343044A CN 201910670036 A CN201910670036 A CN 201910670036A CN 110343044 A CN110343044 A CN 110343044A
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- C07—ORGANIC CHEMISTRY
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- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
Abstract
The invention discloses a kind of synthesizing vinyl acetate ester reaction solution separating technologies.Circulating air is separated and is coupled with product purification, i.e. synthesis gas is introduced into rectifying column after the heavy constituents such as progress rectification process removing acetic acid, crotonaldehyde, after pressurizeing and condensing most of VAC product, acetaldehyde, VAC etc. are absorbed into absorption tower again, the Function Couplings such as rectifying, pressurization condensation, absorption to realize circulating air, are utilized the thermal energy of high-temperature synthesis gas.After pressurization condensation separates condensate liquid, the impurity such as acetaldehyde, acetone, crotonaldehyde, simple flow, energy saving are removed using washing.The invention reside in the separating technologies for redesigning new, and the product purities such as vinylacetate, acetaldehyde and yield can be improved while greatly reducing production energy consumption.
Description
Technical field
The present invention relates to chemical industry rectifying separation field, especially a kind of synthesizing vinyl acetate ester reaction solution separating technology.
Background technique
In the prior art the reaction product of vinyl acetate synthesis kettle mainly include vinylacetate, acetic acid, acetylene, acetaldehyde,
The components such as crotonaldehyde, ethylidene diacetate, acetic anhydride, acetone and water.The gas that 170-230 DEG C of reaction is generated first, warp
While crossing recyclegas knockout tower and realize chilling, using the principle of absorption, by recyclegas acetic acid, acetaldehyde, crotonaldehyde,
The condensations such as ethylidene diacetate, acetic anhydride, acetone and water extraction, into centrifugal station, through a series of isolated VAC of towers, second
The products such as aldehyde, crotonaldehyde, the acetic acid of circulating and recovering and ethylidene diacetate, acetic anhydride etc..
Ma Yangui etc. mentions vinylacetate reaction solution separating technology in " polyvinyl alcohol production technology ", mainly are as follows: follow
Ring gas and reaction, which generate the separation of liquid, to be carried out in recyclegas knockout tower, and upper, middle and lower segment cyclic absorption work is generallyd use
Skill.It is absorbed due to containing acetaldehyde in upper section circulation fluid, and close under conditions of saturation, therefore to the acetaldehyde removal in circulating air
Ability declines to a great extent.In order to improve assimilation effect, will generally control into the temperature of tower top absorbing liquid at 0 DEG C or so, while
The measures such as heavy constituent acetic acid are added in absorbing liquid.While low temperature needs a large amount of freezing energy consumption, out in the circulating air of tower still
So containing substances such as a large amount of VAC, acetaldehyde.The book points out that acetaldehyde has very big adverse effect to reaction system, therefore simultaneously
Circulating air also needs further refinement treatment to remove acetaldehyde, increases a large amount of energy consumption.
In addition the high a large amount of circulation fluid of needs of low boiling point, partial pressure could be removed completely the substances such as acetaldehyde under normal pressure,
This also extremely consumes energy.
Be using another ill-effect that circulation fluid absorbs acetaldehyde: with the progress for absorbing, condensing, absorption tower upper section is inhaled
Liquid is received to increase.Increased portion is distributed to the middle section of recyclegas knockout tower, in lower section circulation fluid in prior art, and then with anti-
Liquid is answered to go out tower.It is such the result is that the substances such as the high crotonaldehyde of acetaldehyde, boiling point of low boiling point and VAC exist simultaneously in reaction solution.
And the influence of acetaldehyde, crotonaldehyde to VAC product quality has very greatly, there is stringent control in VAC product to acetaldehyde, crotonaldehyde
It is required that this just considerably increases the difficulty of VAC product purification, energy consumption of rectification is significantly increased.
And in above-mentioned technique, the separation of circulating air and reaction solution uses the upper, middle and lower of single branch recyclegas knockout tower
Three sections of cyclic absorption techniques.The selection of absorbent, process conditions is set to establish a capital and be restricted really.
In conclusion reaction solution is recycled using simple absorption process in the technique of the vinyl acetate of existing acetylene synthesis,
Energy consumption is high, and impurity makes subsequent separation difficult more in reaction solution.Therefore, a kind of vinyl acetate of acetylene method synthesis is invented in design
Reaction solution separating technology effectively avoids the above problem, improves product index, reduces energy consumption, is to promote vinyl acetate production technique
Key.
Summary of the invention
A kind of gained VAC product purity and product are provided the purpose of the present invention is to solve above-mentioned the deficiencies in the prior art
Matter is high, generated circulation fluid and the high and low energy consumption of circulation gas recovery rate and process flow synthesis vinegar simple to operation in reaction
Vinyl acetate reaction solution separating technology.
To achieve the goals above, the synthesizing vinyl acetate ester reaction solution separating technology designed by the present invention, comprising: circulation
The separation of gas and reaction solution is to be completed twice or repeatedly, and synthesis gas is handled under through different technology conditions twice or repeatedly
After can isolate reaction solution, the reaction system that obtained circulating air can return to synthesizing vinyl acetate ester recycles.Entirely
Reaction system mainly uses rectifying separation, pressurization condensation, absorption processing；The synthesis gas first passes around rectification process and (utilizes height
The thermal energy of warm synthesis gas), heavy constituent acetic acid, acetic anhydride, ethylidene diacetate enter tower bottom liquid phase, and crotons aldehyde is low, and acetic acid can
Direct circulation set uses reaction system；The lights column top row that synthesis gas obtains after rectification process goes out, and is overpressurized, is cooled down
After separating condensate liquid, impurity is removed using washing and directly obtains VAC product, process is simplified, has saved energy consumption of rectification；Without solidifying
Gas absorbs processing through absorption tower again and obtains pure acetylene circulating air Returning reacting system；Impurity in the above process be acetaldehyde,
One of acetone, methyl acetate, crotonaldehyde are a variety of.The absorbent for absorbing processing is that boiling point is higher than 100 DEG C under normal pressure
Solvent, the high boiling component of the appearance during preferably synthetic vinylacetate, i.e. high boiling component are oxalic acid Asia second
One of ester, acetic anhydride, acetic acid are a variety of.
The synthesizing vinyl acetate ester reaction solution separating technology, comprising the following steps:
(1) synthesis gas enters rectifying column T101 progress rectifying separation, obtains liquid from T101 tower bottom and enters next step
(2), fixed gas is obtained to step (3) from T101 tower top；
(2) liquid obtained from T101 tower bottom, containing a small amount of acetic anhydride, ethylidene diacetate, crotons aldehyde is low, can be with
Direct Returning reacting system uses；
(3) fixed gas obtained from T101 tower top is that 130-220kPa is cooled down again by being compressed to gauge pressure, is inhaled into condensation
Tower T102 is received, the fixed gas progress obtained at the top of T102 is rapid (4), and enters T107 in the condensate liquid that the bottom T102 obtains and carry out
Washing, obtains VAC product in the tower top of T107, needs to do electron level VAC product section and enter step (6), the tower bottom of T107 obtains
The aqueous solution containing substances such as acetylene, acetaldehyde, acetone, methyl acetate, VAC, crotonaldehydes arrived enters back into T108 and carries out at rectifying
Reason, the tower top of T111 obtain acetylene, acetaldehyde, methyl acetate, VAC etc. return to T104 processing, the tower bottom of T108 obtain containing acetone,
The aqueous solution of the substances such as crotonaldehyde can be further processed the substances such as recycling acetone, can also directly go waste water station to handle；
(4) T102 fixed gas enters absorption tower T103, and T103 tower top obtains recyclegas acetylene, Returning reacting system set
With, from T102 tower bottom obtain richness-absorbing liquid enter step (5) handle；
(5) T102 tower bottom obtains richness-absorbing liquid and removes the acetylene of dissolution into T104 degassing again, then obtains second into T105 tower top
Aldehyde product, the mixture that T105 tower bottom obtains enter T106, by rectifying separating treatment, obtain acetone, acetic acid in T106 tower top
Methyl esters, VAC etc. are washed into T107, are obtained in T106 tower bottom poor --- and send back in the T103 of absorption tower after absorbent processing and goes to absorb
With.
(6) needing to do electron level VAC product section containing a small amount of water and enter T110 rectifying and dewatering from T107 (or uses drying
Distilled after agent removing moisture), obtain electron level VAC product.
The synthesizing vinyl acetate ester reaction solution separating technology that the present invention obtains, that is, be utilized the thermal energy of high-temperature synthesis gas, into
Row rectifying separates the heavy constituents such as acetic acid, while using the gas cooling of rectifying column, then separates major part by compression, condensation
VAC product finally enters after absorption tower carries out absorption processing and obtains high-purity circulating air acetylene.To realize high-temperature synthesis gas
Effective use, improve condensation, absorption efficiency it is difunctional, the thermal energy of high-temperature synthesis gas is greatly utilized.Integrated artistic stream
Journey is simple to operation, and low energy consumption, and products therefrom purity is high, quality are high, and circulating air utilization rate is high, with high purity.
Detailed description of the invention
Fig. 1 is reaction solution-circulating air separation process schematic diagram of synthesizing vinyl acetate ester reaction solution separating technology.
In Fig. 1: T101- rectifying column, T102- condensed absorbent tower, the absorption tower T103-, T104- take off acetylene tower, T105- acetaldehyde
Tower, T106- lightness-removing column, T107- water scrubber, T108- Product recycling tower, C101 compressor, E101 heat exchanger.
Fig. 2 is the VAC product separation process schematic diagram of synthesizing vinyl acetate ester reaction solution separating technology.
In Fig. 2: T1001- rectifying column, the absorption tower T1002-, the thick VAC tower of T1003-, T1004- crotonaldehyde tower, T1005- vinegar
Acid tower, T1006- lightness-removing column, T1007- acetaldehyde tower, T1008-VAC finishing column, C1001 compressor, E1001 heat exchanger, V1001
Gas-liquid separator, T1010 finishing column, T1011- acetaldehyde tower, T1012- acetone tower.
Specific embodiment
Here is that the invention will be further described in conjunction with attached drawing and by specific embodiment, and following embodiment only describes
Property, it is not restrictive, this does not limit the scope of protection of the present invention.
Embodiment 1: in this example, process flow carries out referring to Fig.1.
(1) synthesis gas enters rectifying column T101 progress rectifying separation, obtains liquid from T101 tower bottom and enters next step
(2), fixed gas is obtained to step (3) from T101 tower top；
(2) liquid obtained from T101 tower bottom, containing a small amount of acetic anhydride, ethylidene diacetate, crotons aldehyde is low, can be with
Direct Returning reacting system uses；
(3) fixed gas obtained from T101 tower top is that 130-220kPa is cooled down again by being compressed to gauge pressure, is inhaled into condensation
Tower T102 is received, the fixed gas progress obtained at the top of T102 is rapid (4), and enters T107 in the condensate liquid that the bottom T102 obtains and carry out
Washing obtains VAC product in the tower top of T107, the tower bottom of T107 obtain containing acetylene, acetaldehyde, acetone, methyl acetate, VAC, bar
The aqueous solution of the substances such as beans aldehyde, enter back into T108 carry out rectification process, the tower top of T108 obtain acetylene, acetaldehyde, methyl acetate,
VAC etc. is returned to T104 and is handled, and the tower bottom of T108 obtains the aqueous solution containing substances such as acetone, crotonaldehydes, can be further processed recycling
The substances such as acetone can also directly go waste water station to handle；
(4) T102 fixed gas enters absorption tower T103, and T103 tower top obtains recyclegas acetylene, Returning reacting system set
With, from T102 tower bottom obtain richness-absorbing liquid enter step (5) handle；
(5) T102 tower bottom obtains richness-absorbing liquid and removes the acetylene of dissolution into T104 degassing again, then obtains second into T105 tower top
Aldehyde product, the mixture that T105 tower bottom obtains enter T106, by rectifying separating treatment, obtain acetone, acetic acid in T106 tower top
Methyl esters, VAC etc. are washed into T107, are obtained in T106 tower bottom poor --- and send back in the T103 of absorption tower after absorbent processing and goes to absorb
With.
(6) needing to do electron level VAC product section containing a small amount of water and enter T110 rectifying and dewatering from T107 (or uses drying
Distilled after agent removing moisture), obtain electron level VAC product.
190 DEG C of the synthesis gas that the synthesis reactor of vinylacetate comes out, into T101 rectifying, rectifying the results are shown in Table 1-1.
Table 1-1
Obtaining liquid from T101 tower bottom is high-purity acetic acid, can directly Returning reacting system apply.
T101 fixed gas enters compressor C101 boosting, obtains condensate liquid and fixed gas into absorption condensation tower T102, ties
Fruit is shown in Table 1-2.
Table 1-2
Absorption condensation tower T102 obtains the efflux that condensate liquid and T106 set come and merges, and is washed to obtain into T107
VAC product 11398kg/h goes out device.It needs to do electron level VAC product section to be dehydrated into T110, electron level VAC is obtained after dehydration
Product the results are shown in Table 1-3.
Table 1-3
Absorption condensation tower T107 obtains water phase and is de-gassed rectifying into T108, the results are shown in Table 1-4.
Table 1-4
Acetone 549kg/h, waste water 18010kg/h, T1080 tower top are obtained after the Produced Liquid rectification process of the bottom T108 using conjunction
And it is further processed into T104.
Embodiment 2:
As shown in Fig. 2, synthesizing vinyl acetate ester reaction solution separating technology provided by the invention, comprising: circulating air with react
The separation of liquid is to be completed twice or repeatedly, and synthesis gas can divide after handling under different technology conditions twice or repeatedly
Reaction solution is separated out, the reaction system that obtained circulating air can return to synthesizing vinyl acetate ester recycles.Entire reaction system
Mainly using rectifying separation, pressurization condensation, absorption processing；The synthesis gas first passes around rectification process, the thick VAC of heavy constituent, bar
Beans aldehyde, acetic acid, acetic anhydride, ethylidene diacetate enter tower bottom liquid phase, then are respectively obtained slightly by rectifying separating treatment three times
The mixture of VAC, crotonaldehyde, acetic acid and acetic anhydride and ethylidene diacetate；Obtained after rectification process light group of synthesis gas
Divide tower top of entering, after being overpressurized condensation and separating condensate liquid, impurity is removed using washing, and fixed gas is handled through absorption again；On
Stating impurity is one of acetaldehyde, acetone, crotonaldehyde or a variety of.The absorbent for absorbing processing is that boiling point is higher than under normal pressure
100 DEG C of solvent.Absorbing liquid for absorption tower T1003 is the high boiling component of the appearance during synthesizing vinyl acetate ester.
The high boiling component is one of ethylidene diacetate, acetic anhydride, acetic acid or a variety of.
The synthesizing vinyl acetate ester reaction solution separating technology, comprising the following steps:
(1) synthesis gas enters rectifying column T1001 progress rectifying separation, obtains liquid from T1001 tower bottom and enters next step
(2), fixed gas is obtained to step (3) from T1001 tower top；
(2) enter T1003 from the liquid that T1001 tower bottom obtains and carry out rectifying separation, obtain thick VAC in the tower top of T1003,
T1004 is entered back into the liquid that the tower bottom of T1003 obtains and carries out rectifying separation, crotonaldehyde is obtained in the tower top of T1004, in T1004
The obtained liquid of tower bottom enter T1005 rectification process, obtain acetic acid in the tower top of T1005, obtain acetic anhydride in the tower bottom of T1005
With the mixture of ethylidene diacetate；
(3) fixed gas obtained from T1001 tower top is that 130-220kPa is cooled down again by being compressed to gauge pressure, into gas-liquid point
From device V1001, the fixed gas progress obtained at the top of V1001 is rapid (4), and enters T1010 in the condensate liquid that the bottom V1001 obtains
Rectification process obtains VAC product in the tower top of T1010, and the mixture that the tower bottom of T1010 obtains enters back into T1011 and carries out rectifying
Processing obtains ethyl alcohol in the tower top of T1011, and the mixture that the tower bottom of T1011 obtains enters back into T1012 and carries out rectification process,
T1012 tower top obtains acetone, sends T1010 back to after washed dose of the mixture that T1012 tower bottom obtains processing and carries out rectification process；
(4) V1001 fixed gas enters absorption tower T1002, and T1002 tower top obtains poor-absorbing liquid return T1002 and makees absorbent
It applies, V1001 fixed gas and poor-absorbing liquid from T1002 tower top carry out counter-current absorption, obtain richness-absorption from T1002 tower bottom
Liquid enters step (5) processing；
(5) T1002 tower bottom obtains richness-absorbing liquid again into T1006, and the mixture that T1006 tower top obtains enters T1007,
The mixture that T1006 tower bottom obtains enters T1008, by rectifying separating treatment, ethyl alcohol is obtained in T1007 tower top, in T1007 tower
Bottom obtains acetone, obtains VAC product in T1008 tower top, the mixture that wherein T1008 tower bottom obtains is sent back to after absorbent is handled
Into absorption tower T1002.
The thick VAC can be reprocessed back to T1001, and described and above-mentioned acetic acid, acetic anhydride, ethylidene diacetate are equal
It can cover to use in reaction system and be recycled, the T1002 tower top obtains circulating air, by suitably refining or directly returning to reaction
System is applied.190 DEG C of the synthesis gas that the synthesis reactor of vinylacetate comes out, into T1001 rectifying, rectifying the results are shown in Table 2-1.
Table 2-1
Liquid, which is obtained, from T1001 tower bottom obtains thick VAC 452kg/h, crotons into rectifying such as T1003, T1004, T1005 again
The 62kg/h such as aldehyde product 120kg/h goes out device, acetic acid 10853kg/h return synthesis reaction system is applied, aceticanhydride.
After T1001 fixed gas enters compressor C1001 boosting, heat exchanger E1001 heat exchange, into gas-liquid separator V1001
Condensate liquid and fixed gas are obtained, the results are shown in Table 2-2.
Table 2-2
Separator V1001 obtains condensate liquid through further isolated acetaldehyde 251kg/h, acetone 439kg/h, VAC product
9660.5kg/h device out.
Separator V1001 obtains fixed gas and is absorbed into T1002, and comes from 10 DEG C of tower top temperature, and flow is
The acetic acid aqueous solution that 50000kg/h concentration is 80% carries out counter-current absorption, the results are shown in Table 2-3.
Table 2-3
The bottom T1002 Produced Liquid obtains acetaldehyde 316kg/ into T1006 rectifying after the rectification process such as T1007, T1008
H, acetone 115kg/h, VAC product 1376kg/h recycles absorbent acetic acid+50.08 tons/h of water.
Embodiment 3: in this example, carrying out referring to process flow diagram 2, what the synthesis reactor of vinylacetate came out
190 DEG C of synthesis gas, into T1001 rectifying, rectifying the results are shown in Table 3-1.
Table 3-1
Obtaining liquid from T1001 tower bottom is acetic acid (acetaldehyde 0.009%, the vinegar that crotons aldehyde is 0.006%
Acid), it directly returns to synthesis reaction system and applies.
After T1001 fixed gas enters compressor C1001 boosting, heat exchanger E1001 heat exchange, into gas-liquid separator V1001
Condensate liquid and fixed gas are obtained, the results are shown in Table 3-2.
Table 3-2
Separator V1001 obtain condensate liquid through washing etc. further isolated acetaldehyde 263kg/h, acetone 451kg/h,
VAC product 10102.5kg/h, acetic acid 700kg/h, crotonaldehyde 33kg/h go out device, the results are shown in Table 3-3.
Table 3-3
The bottom T1002 Produced Liquid obtains acetaldehyde 265kg/ into T1006 rectifying after the rectification process such as T1007, T1008
H, acetone 105kg/h, VAC product 1249kg/h recycles 50.06 tons/h of absorbent ethylene glycol diacetate.
Claims (7)
1. a kind of synthesizing vinyl acetate ester reaction solution separating technology, it is characterised in that: the separation of circulating air and reaction solution is through two
Secondary or repeatedly complete, synthesis gas can isolate reaction solution after handling under different technology conditions twice or repeatedly, obtain
To circulating air return synthesizing vinyl acetate ester reaction system recycle.
2. synthesizing vinyl acetate ester reaction solution separating technology described in one kind according to claim 1, it is characterised in that: anti-
Synthesis gas is answered mainly to use rectifying separation, pressurization condensation, absorption processing；The synthesis gas first with high-temperature synthesis gas thermal energy
By rectification process, heavy constituent acetic acid, acetic anhydride, ethylidene diacetate enter tower bottom liquid phase；Synthesis gas obtains after rectification process
To light component enter tower top, after being overpressurized condensation and separating condensate liquid, impurity is removed using washing, and fixed gas is again through absorbing
Processing；Above-mentioned impurity is one of acetaldehyde, acetone, methyl acetate, crotonaldehyde or a variety of.
3. a kind of synthesizing vinyl acetate ester reaction solution separating technology according to claim 2, it is characterised in that: remove acetic acid
Etc. liquid containing VAC after heavy constituents, VAC product can be obtained by washing, can also by washing and being dehydrated, rectifying obtain it is high
The VAC product of purity.
4. synthesizing vinyl acetate ester reaction solution separating technology described in one kind according to claim 2, it is characterised in that: institute
State solvent of the absorbent for absorbing processing for boiling point under normal pressure higher than 100 DEG C.
5. synthesizing vinyl acetate ester reaction solution separating technology described in one kind according to claim 2, it is characterised in that: institute
Stating high boiling component is one of ethylidene diacetate, acetic anhydride, acetic acid or a variety of.
6. synthesizing vinyl acetate ester reaction solution separating technology described in one kind described in -5 according to claim 1, it is characterized in that packet
Include following steps:
(1) synthesis gas enters rectifying column T101 progress rectifying separation, obtains liquid from T101 tower bottom and enters next step (2), from
T101 tower top obtains fixed gas to step (3)；
(2) liquid obtained from T101 tower bottom, containing a small amount of acetic anhydride, ethylidene diacetate, crotons aldehyde is low, can be direct
Returning reacting system uses；
(3) fixed gas obtained from T101 tower top is that 130-220kPa is cooled down again by being compressed to gauge pressure, into condensed absorbent tower
T102, the fixed gas progress obtained at the top of T102 is rapid (4), and enters T107 in the condensate liquid that the bottom T102 obtains and carry out water
It washes, obtains VAC product in the tower top of T107, need to do electron level VAC product section and enter step (6), the tower bottom of T107 obtains
The aqueous solution containing substances such as acetylene, acetaldehyde, acetone, methyl acetate, VAC, crotonaldehydes, enter back into T108 carry out rectification process,
The tower top of T111 obtain acetylene, acetaldehyde, methyl acetate, VAC etc. return to T104 processing, the tower bottom of T108 obtain containing acetone, bar
The aqueous solution of the substances such as beans aldehyde can be further processed the substances such as recycling acetone, can also directly go waste water station to handle；
(4) T102 fixed gas enters absorption tower T103, and T103 tower top obtains recyclegas acetylene, and Returning reacting system is applied, from
T102 tower bottom obtains richness-absorbing liquid and enters step (5) processing；
(5) T102 tower bottom obtains richness-absorbing liquid and removes the acetylene of dissolution into T104 degassing again, then obtains acetaldehyde into T105 tower top and produce
Product, the mixture that T105 tower bottom obtains enter T106, by rectifying separating treatment, T106 tower top obtain acetone, methyl acetate,
VAC etc. is washed into T107, is obtained in T106 tower bottom poor --- and send back in the T103 of absorption tower to go to absorb after absorbent processing and use.
From T107 containing a small amount of water need to do electron level VAC product section enter T110 rectifying and dewatering or with desiccant remove water
It is distilled after point, obtains electron level VAC product.
7. synthesizing vinyl acetate ester reaction solution separating technology described in one kind according to claim 5, it is characterised in that: use
In absorption tower T103 absorbing liquid be synthesizing vinyl acetate ester during appearance high boiling component.
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| CN113861026A (en) * | 2021-10-29 | 2021-12-31 | 天津大学 | Refining method of vinyl acetate and acetic acid synthesized by acetylene method |
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Application publication date: 20191018 |