CN207987066U - A kind of device of synthesizing methyl acrylic anhydride - Google Patents
A kind of device of synthesizing methyl acrylic anhydride Download PDFInfo
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- CN207987066U CN207987066U CN201820125553.3U CN201820125553U CN207987066U CN 207987066 U CN207987066 U CN 207987066U CN 201820125553 U CN201820125553 U CN 201820125553U CN 207987066 U CN207987066 U CN 207987066U
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- Prior art keywords
- discharge port
- anhydride
- feed inlet
- methacrylic
- acetic acid
- Prior art date
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- DCUFMVPCXCSVNP-UHFFFAOYSA-N methacrylic anhydride Chemical compound CC(=C)C(=O)OC(=O)C(C)=C DCUFMVPCXCSVNP-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 26
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 257
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims abstract description 174
- 238000006243 chemical reaction Methods 0.000 claims abstract description 84
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 70
- 238000000066 reactive distillation Methods 0.000 claims abstract description 43
- 238000010992 reflux Methods 0.000 claims abstract description 42
- 239000003112 inhibitor Substances 0.000 claims abstract description 32
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 31
- 239000000945 filler Substances 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims description 3
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 3
- 208000012839 conversion disease Diseases 0.000 abstract description 7
- 238000009835 boiling Methods 0.000 description 14
- 238000004519 manufacturing process Methods 0.000 description 13
- 238000000034 method Methods 0.000 description 11
- 150000008065 acid anhydrides Chemical class 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 239000006227 byproduct Substances 0.000 description 7
- 239000012043 crude product Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 6
- 235000010354 butylated hydroxytoluene Nutrition 0.000 description 6
- 238000000889 atomisation Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000010924 continuous production Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005194 fractionation Methods 0.000 description 3
- 238000010025 steaming Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000012644 addition polymerization Methods 0.000 description 2
- IAQRGUVFOMOMEM-UHFFFAOYSA-N but-2-ene Chemical group CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- -1 methacrylic acid thioesters Chemical class 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 150000001896 cresols Chemical class 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- ARJOQCYCJMAIFR-UHFFFAOYSA-N prop-2-enoyl prop-2-enoate Chemical compound C=CC(=O)OC(=O)C=C ARJOQCYCJMAIFR-UHFFFAOYSA-N 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003509 tertiary alcohols Chemical class 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of device of synthesizing methyl acrylic anhydride, including：Reactive distillation column；The middle part of the reactive distillation column includes reaction zone and the rectification zone positioned at the both sides up and down of the reaction zone, and tower top is equipped with acetic acid discharge port and filler entrance, and bottom of tower is equipped with methacrylic anhydride tower reactor；The reaction zone is equipped with methacrylic acid feed inlet, acetic anhydride feed inlet and steam-heating system；The First Heat Exchanger that discharge port is connected with the methacrylic acid feed inlet；The second heat exchanger that discharge port is connected with the acetic anhydride feed inlet；The condenser that feed inlet is connected with the acetic acid discharge port；The condenser is equipped with vacuum plant；The return tank that feed inlet is connected with the discharge port of the condenser；The return tank, which is equipped with acetic acid and exports and flow back, expects outlet；Reflux material outlet is connected through reflux pump and return line with the filler entrance successively；The polymerization inhibitor tank that discharge port is communicated with the return line.The device can realize continuous reaction rectification, and reaction conversion ratio is high, product quality is stablized.
Description
Technical field
The utility model is related to organic synthesis technical fields, are to be related to a kind of synthesizing methyl acrylic acid more specifically
The device of acid anhydride.
Background technology
Methacrylic anhydride is a kind of stronger esterifying agent, is to prepare methacrylic acid thioesters, Methacrylamide and first
Reagent necessary to base acrylate (the especially ester of the tertiary alcohol) is applied at the same time as polymerisation crosslinking agent for photocuring
The synthesis of the materials such as material, crosslinked resin also can be used as synthesis of the raw material for extraordinary fine chemicals, have a vast market and answer
Use foreground.
Currently, the technique of synthesizing methyl acrylic anhydride disclosed in the prior art is broadly divided into two classes：The first kind is first to synthesize
Reaction waits starting rectifying after the completion of reacting；Second class is intermittent reaction rectifying, the rectifying simultaneously during reaction.Due to
First kind synthetic reaction production efficiency is low, high energy consumption, by-product are higher, generally uses the interval of the second class in actual production
Formula reactive distillation synthesizing methyl acrylic anhydride.Although the second class batch reactive distillation technique is carried compared with first kind method efficiency
Height, but batch production mode cannot be overcome always, production efficiency and energy consumption are still higher, easy to produce by-product, are not suitable for
In industrialized production.
Utility model content
In view of this, the purpose of this utility model is to provide a kind of device of synthesizing methyl acrylic anhydride, can realize
Continuous reaction rectification, and reaction conversion ratio is high, product quality is stablized.
The utility model provides a kind of device of synthesizing methyl acrylic anhydride, including：
Reactive distillation column；The middle part of the reactive distillation column includes reaction zone and the both sides up and down positioned at the reaction zone
Rectification zone, tower top are equipped with acetic acid discharge port and filler entrance, and bottom of tower is equipped with methacrylic anhydride tower reactor；The reaction zone is equipped with first
Base acrylic acid feed inlet, acetic anhydride feed inlet and steam-heating system；
The First Heat Exchanger that discharge port is connected with the methacrylic acid feed inlet；
The second heat exchanger that discharge port is connected with the acetic anhydride feed inlet；
The condenser that feed inlet is connected with the acetic acid discharge port；The condenser is equipped with vacuum plant；
The return tank that feed inlet is connected with the discharge port of the condenser；The return tank, which is equipped with acetic acid and exports and flow back, expects
Outlet；Reflux material outlet is connected through reflux pump and return line with the filler entrance successively；
The polymerization inhibitor tank that discharge port is communicated with the return line.
Preferably, the methacrylic acid feed inlet is equipped with atomizer.
Preferably, the acetic anhydride feed inlet is equipped with atomizer.
Preferably, filler is used in the rectification zone；The filler is in structured packing, Raschig ring and the poly- saddle ring of Pall ring
It is one or more.
Preferably, the methacrylic anhydride tower reactor is equipped with steam-heating system, in-line analyzer and methacrylic anhydride
Outlet.
Preferably, the theoretical cam curve of the reactive distillation column is 10~35.
Preferably, the discharge port of the First Heat Exchanger is equipped with temperature control equipment, volume control device and valve.
Preferably, the discharge port of second heat exchanger is equipped with temperature control equipment, volume control device and valve.
Preferably, the condenser is equipped with in-line analyzer.
Preferably, the vacuum plant includes：
The vacuum tube communicated with the condenser；
The vacuum pump communicated with the vacuum tube.
The utility model provides a kind of device of synthesizing methyl acrylic anhydride, including：Reactive distillation column；The reaction essence
The middle part for evaporating tower includes reaction zone and the rectification zone positioned at the both sides up and down of the reaction zone, and tower top is equipped with acetic acid discharge port and fills out
Expect that entrance, bottom of tower are equipped with methacrylic anhydride tower reactor；The reaction zone be equipped with methacrylic acid feed inlet, acetic anhydride feed inlet and
Steam-heating system；The First Heat Exchanger that discharge port is connected with the methacrylic acid feed inlet；Discharge port and the acetic anhydride
The second connected heat exchanger of feed inlet；The condenser that feed inlet is connected with the acetic acid discharge port；The condenser is equipped with vacuum
Device；The return tank that feed inlet is connected with the discharge port of the condenser；The return tank is equipped with acetic acid outlet and reflux expects
Mouthful；Reflux material outlet is connected through reflux pump and return line with the filler entrance successively；Discharge port and the return duct
The polymerization inhibitor tank that road communicates.Compared with prior art, the device of synthesizing methyl acrylic anhydride provided by the utility model can be real
Existing continuous reaction rectification, production efficiency are high；And reaction conversion ratio is high, product quality is stablized.The experimental results showed that this practicality is new
The conversion ratio of the raw material methacrylic acid for the device synthesizing methyl acrylic anhydride that type provides is 99% or more, and product yield is 90%
More than, purity is 95% or more.
In addition, the device of synthesizing methyl acrylic anhydride provided by the utility model can also access high-purity acetic acid, and its
His by-product is extremely low, meets environmental requirement；Simultaneously can continuous production, be easy to implement industrialization, automated production, adapt to epoch hair
Exhibition needs.
Description of the drawings
Fig. 1 is the structural schematic diagram of the device for the synthesizing methyl acrylic anhydride that the utility model embodiment provides.
Specific implementation mode
Below in conjunction with the utility model embodiment, the technical solution of the utility model is clearly and completely described,
Obviously, the described embodiments are only a part of the embodiments of the utility model, instead of all the embodiments.Based on this practicality
Embodiment in novel, every other reality obtained by those of ordinary skill in the art without making creative efforts
Example is applied, shall fall within the protection scope of the present invention.
The utility model provides a kind of device of synthesizing methyl acrylic anhydride, including：
Reactive distillation column；The middle part of the reactive distillation column includes reaction zone and the both sides up and down positioned at the reaction zone
Rectification zone, tower top are equipped with acetic acid discharge port and filler entrance, and bottom of tower is equipped with methacrylic anhydride tower reactor；The reaction zone is equipped with first
Base acrylic acid feed inlet, acetic anhydride feed inlet and steam-heating system；
The First Heat Exchanger that discharge port is connected with the methacrylic acid feed inlet；
The second heat exchanger that discharge port is connected with the acetic anhydride feed inlet；
The condenser that feed inlet is connected with the acetic acid discharge port；The condenser is equipped with vacuum plant；
The return tank that feed inlet is connected with the discharge port of the condenser；The return tank, which is equipped with acetic acid and exports and flow back, expects
Outlet；Reflux material outlet is connected through reflux pump and return line with the filler entrance successively；
The polymerization inhibitor tank that discharge port is communicated with the return line.
In the present invention, the device of the synthesizing methyl acrylic anhydride includes reactive distillation column, First Heat Exchanger,
Two heat exchangers, condenser, return tank and polymerization inhibitor tank.Referring to Fig. 1, Fig. 1 is the synthesis first that the utility model embodiment provides
The structural schematic diagram of the device of base acrylic anhydride.Wherein, 01 is First Heat Exchanger, and 02 is the second heat exchanger, and 03 is condenser, 04
It is return tank for reactive distillation column, 05,06 is polymerization inhibitor tank.
In the present invention, the middle part of the reactive distillation column includes reaction zone and positioned at up and down the two of the reaction zone
The rectification zone of side.In the present invention, the reaction zone is used for the mixing and reaction of methacrylic acid and acetic anhydride；It is described anti-
Area is answered to be equipped with methacrylic acid feed inlet, acetic anhydride feed inlet and steam-heating system；Wherein, the methacrylic acid feed inlet
For the charging of methacrylic acid, the acetic anhydride feed inlet is used for the charging of acetic anhydride, and the steam-heating system is for controlling
Reaction temperature processed.
In the present invention, the methacrylic acid feed inlet is preferably provided with atomizer；The acetic anhydride feed inlet is excellent
Choosing is equipped with atomizer.Methacrylic acid and acetic anhydride are atomized by the utility model using atomizer, make methacrylic acid and
Atomization contact is realized in the mixing of acetic anhydride, to ensure that reaction raw materials come into full contact with.
In the present invention, the rectification zone is located at the both sides up and down of the reaction zone；Wherein, it is located at the reaction zone
The low-boiling acetic acid crude product that the rectification zone of upside is used to obtain after being reacted the reaction zone carries out rectifying, is located at described
The high boiling methacrylic anhydride crude product that rectification zone on the downside of reaction zone is used to obtain after being reacted the reaction zone into
Row rectifying.In the present invention, filler is preferably used in the rectification zone；The filler is preferably structured packing, Raschig ring
With it is one or more in the poly- saddle ring of Pall ring；It is not specifically limited to this for the utility model.
In the present invention, the tower top of the reactive distillation column is equipped with acetic acid discharge port and filler entrance；Wherein, described
Acetic acid discharge port flows back for the reactive distillation column to be discharged in acetic acid, the filler entrance be used to flow back after acetic acid and
The charging of polymerization inhibitor.
In the present invention, the bottom of tower of the reactive distillation column is equipped with methacrylic anhydride tower reactor.In the utility model
In, the methacrylic anhydride tower reactor is preferably provided with steam-heating system, in-line analyzer and methacrylic anhydride outlet；Its
In, the steam-heating system is used to the methacrylic anhydride in the methacrylic anhydride tower reactor carrying out steam heating, into
One step excludes wherein minute quantity light substance, and the in-line analyzer is used to judge whether methacrylic anhydride reaches criterion of acceptability,
The methacrylic anhydride outlet reaches the methacrylic anhydride of criterion of acceptability for output.
In the present invention, the theoretical cam curve of the reactive distillation column is preferably 10~35.
In the present invention, the First Heat Exchanger is for preheating raw material methacrylic acid.It is new in this practicality
In type, the First Heat Exchanger is equipped with methacrylic acid entrance and discharge port；Wherein, the methacrylic acid entrance is used for methyl
The charging of acrylic acid, discharging of the discharge port for the methacrylic acid after preheating.In the present invention, it described first changes
The discharge port of hot device is connected with the methacrylic acid feed inlet.
In the present invention, the discharge port of the First Heat Exchanger is preferably provided with temperature control equipment, flow control dress
It sets and valve；Wherein, the temperature control equipment is used to control the preheating temperature of methacrylic acid, and the volume control device is logical
Unlatching/the closing for controlling the valve is crossed, the feed rate of methacrylic acid is adjusted.
In the present invention, second heat exchanger is for preheating raw acetic acid acid anhydride.In the present invention,
Second heat exchanger is equipped with acetic anhydride entrance and discharge port；Wherein, the acetic anhydride entrance is used for the charging of acetic anhydride, described
Discharging of the discharge port for the acetic anhydride after preheating.In the present invention, the discharge port of second heat exchanger and the second
Anhydride charge mouth is connected.
In the present invention, the discharge port of second heat exchanger is preferably provided with temperature control equipment, flow control dress
It sets and valve；Wherein, the temperature control equipment is used to control the preheating temperature of acetic anhydride, and the volume control device passes through control
Unlatching/the closing for making the valve, adjusts the feed rate of acetic anhydride.
In the present invention, the condenser is for condensing the acetic acid that the acetic acid discharge port is discharged.At this
In utility model, the condenser is equipped with feed inlet, vacuum plant, discharge port and in-line analyzer；Wherein, the feed inlet with
The acetic acid discharge port is connected, and the vacuum plant is used to control the vacuum degree in the reactive distillation column, and the discharge port is used
In condensed acetic acid is discharged, the in-line analyzer is for judging whether acetic acid reaches criterion of acceptability.
In the present invention, the vacuum plant preferably includes vacuum tube and vacuum pump；Wherein, the vacuum tube and institute
It states condenser to communicate, the vacuum pump is communicated with the vacuum tube.The utility model is controlled described anti-by the vacuum plant
Negative pressure in rectifying column (i.e. vacuum degree) is answered, to which raw material methacrylic acid and acetic anhydride are sucked the reactive distillation column.
In the present invention, the return tank is equipped with feed inlet, acetic acid outlet and the outlet of reflux material；Wherein, it is described into
Material mouth is connected with the discharge port of the condenser, and the acetic acid outlet reaches the acetic acid of criterion of acceptability, the reflux for output
Acetic acid of the material outlet for reflux to be discharged.
In the present invention, reflux material outlet is successively through reflux pump and return line and the filler entrance phase
Even.In the present invention, for the reflux pump for pressurizeing to acetic acid, the acetic acid after pressurization is back to institute through return line
State filler entrance.
In the present invention, the polymerization inhibitor tank is equipped with discharge port and valve；Wherein, the discharge port and the reflux
Pipeline communicates, and the valve is for opening/closing the discharge port.In the present invention, polymerization inhibitor is in the return line
In mixed with acetic acid, through acetic acid enter the filler entrance；Since polymerization inhibitor boiling point is higher, can be down to by tower top described
Methacrylic anhydride tower reactor.
In the present invention, the polymerization inhibitor is preferably selected from 2,6-di-tert-butyl p-cresol and/or phenthazine；This practicality
The novel source to the polymerization inhibitor is not particularly limited, using above-mentioned 2,6- di-t-butyls pair well known to those skilled in the art
The commercial goods of cresols and phenthazine.In the present invention, the polymerization inhibitor can effectively avoid the reactive distillation
Polymerization in tower.
The device of synthesizing methyl acrylic anhydride provided by the utility model by continuous feed, continuous reaction rectification, return again
Stream, realizes continuous output acetic acid and methacrylic anhydride, while entire technique being made to tend towards stability, and can realize successive reaction essence
It evaporates, production efficiency is high；And reaction conversion ratio is high, product quality is stablized.In addition, synthesizing methyl propylene provided by the utility model
The device of acid anhydrides can obtain high-purity acetic acid, and other by-products are extremely low, meet environmental requirement；Simultaneously can continuous production, just
In realizing industrialization, automated production, adapts to era development and need.
The utility model additionally provides a kind of method of synthesizing methyl acrylic anhydride, includes the following steps：
A) it mixes after preheating methacrylic acid and acetic anhydride respectively, is reacted under vacuum, then rectifying, respectively obtain
Acetic acid and methacrylic anhydride；
B) it mixes, flows back with polymerization inhibitor after condensing the acetic acid that step a) is obtained, the methyl-prop obtained with step a)
Olefin(e) acid acid anhydride mixes, continuous output methacrylic anhydride after stablizing.
The utility model mixes after first preheating methacrylic acid and acetic anhydride respectively, is reacted under vacuum, then
Rectifying respectively obtains acetic acid and methacrylic anhydride.The utility model is using methacrylic acid and acetic anhydride as Material synthesis methyl
Acrylic anhydride；The utility model is not particularly limited the source of the methacrylic acid and acetic anhydride, using art technology
Commercial goods known to personnel.
In the present invention, the preheating temperature of the methacrylic acid is preferably 85 DEG C~105 DEG C, more preferably 90 DEG C
~100 DEG C.In the present invention, the preheating temperature of the acetic anhydride is preferably 75 DEG C~100 DEG C, more preferably 80 DEG C~90
℃。
In the present invention, the mode of the mixing is preferably atomized contact；The utility model is using atomization contact
Mode mixes methacrylic acid and acetic anhydride, ensures that reaction raw materials come into full contact with.
In the present invention, during the mixing, the inlet amount of methacrylic acid and acetic anhydride is preferably using double
Closed loop becomes ratio servo antrol；Methacrylic acid is 2 with acetic anhydride charging reaction ratio theoretical value：1, since the reaction is reversible
Reaction carries out in order to avoid reacting reverse, therefore ingredient proportion is slightly larger than theoretical proportions, is carried out in order to react to positive direction.
In the present invention, the feed rate of the methacrylic acid and acetic anhydride ratio is preferably (2.0~2.8)：1.
Meanwhile the separated from acetic acid that will be obtained after reaction, make reaction balance to positive direction carry out, improve reaction conversion ratio and
Yield；The acetic acid obtained after reaction after analysis is qualified, and feeds and flows back and tend to stable state, and the charging proportioning of reaction uses institute
The content that two close cycles become ratio servo antrol methacrylic acid is stated, when containing methacrylic acid in methacrylic anhydride, is used
The two close cycles become ratio servo antrol and gradually reduce base acrylic acid and acetic anhydride inlet amount ratio, close to theoretical value 2：1, when
When the methacrylic acid contained in methacrylic anhydride reaches criterion of acceptability, methacrylic acid and acetic anhydride feed rate ratio become
In stabilization.
In the present invention, the temperature of the reaction is preferably 75 DEG C~115 DEG C, more preferably 90 DEG C~100 DEG C；Institute
The vacuum degree for stating reaction is preferably -7KPa~-15KPa, more preferably -10KPa~-12KPa.The utility model is in vacuum condition
Under, on the one hand byproduct of reaction can be made to be detached from reaction system in time, on the other hand reduce metering system obtained by the reaction
To reduce it possibility of polymerisation occurs for the temperature of acid anhydrides.
In the present invention, the low-boiling acetic acid crude product and height boiling that the process of the rectifying will obtain after reaction respectively
The methacrylic anhydride crude product of point carries out rectifying, respectively obtains acetic acid and methacrylic anhydride.
After respectively obtaining the acetic acid and methacrylic anhydride, the utility model by obtained acetic acid condense after with polymerization inhibitor
Mixing, flows back, is mixed with the obtained methacrylic anhydrides of step a), continuous output methacrylic anhydride after stablizing.At this
In utility model, the polymerization inhibitor is preferably selected from 2,6-di-tert-butyl p-cresol and/or phenthazine.The utility model is to the resistance
The source of poly- agent is not particularly limited, using above-mentioned 2,6-di-tert-butyl p-cresol well known to those skilled in the art and phenthazine
Commercial goods.In the present invention, the polymerization inhibitor can effectively prevent the polymerisation of methacrylic acid.
In the present invention, the reflux ratio of the reflux is preferably 1：(1.5~3.5), more preferably 1：(2~3).
In the utility model, the reflux ratio is the mass ratio of the acetic acid to flow back and the acetic acid obtained in step a).The utility model
It is preferred that further including：
By condensed acetic acid output, acetic acid product is obtained.In the actual production process, acetic acid is in addition to reflux, additionally it is possible to
The acetic acid product of criterion of acceptability must be reached, it is not specifically limited to this for the utility model.
In the present invention, the theoretical cam curve after the stabilization is preferably 10~35.
In the present invention, the step b) preferably further includes：
Methacrylic anhydride before output is subjected to steam heating.In the present invention, the steam-heated purpose
It is minute quantity light substance in further exclusion methacrylic anhydride, it is not specifically limited to this for the utility model.
The method of synthesizing methyl acrylic anhydride provided by the utility model by continuous feed, continuous reaction rectification, return again
Stream, realizes continuous output acetic acid and methacrylic anhydride, while entire technique being made to tend towards stability, and can realize successive reaction essence
It evaporates, production efficiency is high；And reaction conversion ratio is high, product quality is stablized.In addition, synthesizing methyl propylene provided by the utility model
The device of acid anhydrides can obtain high-purity acetic acid, and other by-products are extremely low, meet environmental requirement；Simultaneously can continuous production, just
In realizing industrialization, automated production, adapts to era development and need.
The utility model provides a kind of device of synthesizing methyl acrylic anhydride, including：Reactive distillation column；The reaction essence
The middle part for evaporating tower includes reaction zone and the rectification zone positioned at the both sides up and down of the reaction zone, and tower top is equipped with acetic acid discharge port and fills out
Expect that entrance, bottom of tower are equipped with methacrylic anhydride tower reactor；The reaction zone be equipped with methacrylic acid feed inlet, acetic anhydride feed inlet and
Steam-heating system；The First Heat Exchanger that discharge port is connected with the methacrylic acid feed inlet；Discharge port and the acetic anhydride
The second connected heat exchanger of feed inlet；The condenser that feed inlet is connected with the acetic acid discharge port；The condenser is equipped with vacuum
Device；The return tank that feed inlet is connected with the discharge port of the condenser；The return tank is equipped with acetic acid outlet and reflux expects
Mouthful；Reflux material outlet is connected through reflux pump and return line with the filler entrance successively；Discharge port and the return duct
The polymerization inhibitor tank that road communicates.Compared with prior art, the device of synthesizing methyl acrylic anhydride provided by the utility model can be real
Existing continuous reaction rectification, production efficiency are high；And reaction conversion ratio is high, product quality is stablized.The experimental results showed that this practicality is new
Type provides the conversion ratio of the raw material methacrylic acid of the synthesizing methyl acrylic anhydride of device 99% or more, and product yield is 90%
More than, purity is 95% or more.
In addition, the device of synthesizing methyl acrylic anhydride provided by the utility model can also access high-purity acetic acid, and its
His by-product is extremely low, meets environmental requirement；Simultaneously can continuous production, be easy to implement industrialization, automated production, adapt to epoch hair
Exhibition needs.
In order to further illustrate the utility model, it is described in detail below by following embodiment.The utility model with
The structural schematic diagram of the device of synthesizing methyl acrylic anhydride used in lower embodiment is shown in Figure 1；Wherein, 01 is the first heat exchange
Device, 011 is temperature control equipment, and 012 is volume control device, and 013 is valve, and 014 is methacrylic acid entrance, and 02 is second
Heat exchanger, 021 is temperature control equipment, and 022 is volume control device, and 023 is valve, and 024 is acetic anhydride entrance, and 03 is condensation
Device, 031 is in-line analyzer, and 032 is vacuum tube, and 04 is reactive distillation column, and 041 is reaction zone, and 042 is methacrylic anhydride tower
Kettle, 043 is rectification zone, and 044 is in-line analyzer, and 045 is atomizer, and 046 exports for methacrylic anhydride, and 05 is return tank,
051 exports for acetic acid, and 06 is polymerization inhibitor tank, and 07 is reflux pump.
Embodiment 1
(1) methacrylic acid is preheated in methacrylic acid entrance (014) into First Heat Exchanger (01), is led to after preheating
Control temperature control equipment (011) is crossed controlled at 95 DEG C, into reactive distillation column (04), is kept in reactive distillation column (04)
Vacuum degree -11KPa, methacrylic acid is interior by the interior negative pressure sucting reaction rectifying column (04) of reactive distillation column (04), and passes through mist
Change device (045) to be atomized；Acetic anhydride is preheated in acetic anhydride entrance (024) into the second heat exchanger (02) simultaneously, is preheated
Afterwards by controlling temperature control equipment (021) controlled at 85 DEG C, into reactive distillation column (04), acetic anhydride is by reacting essence
It evaporates in tower in negative pressure sucting reaction rectifying column (04), and be atomized by the atomizer (045) in tower, realizes methacrylic acid
Atomization with acetic anhydride contacts.
(2) feed rate that methacrylic acid is controlled by volume control device (012), passes through volume control device
(022) feed rate for controlling methacrylic acid, it is 2.4 to make the feed rate of the methacrylic acid and acetic anhydride ratio：1；Institute
It states methacrylic acid and acetic anhydride to be reacted in reaction zone (041), the reaction zone (041) is kept by steam-heating system
Reaction temperature keeps vacuum degree -11KPa at 90 DEG C~100 DEG C；The low-boiling acetic acid crude product generated is reacted directly to described
Rectification zone (043) obtains acetic acid to top fractionation on the upside of reaction zone (041)；React the high boiling methacrylic anhydride generated
It obtains methacrylic anhydride to bottom rectifying through rectification zone (043) on the upside of the reaction zone (041) and enters methacrylic anhydride tower
Kettle (042).
(3) after the acetic acid that step (2) obtains at the top of the reactive distillation column (04) by steaming, condensed device (03) cooling is cold
After solidifying, into return tank (05), control reflux ratio is 1：2.5, will for the acetic acid of reflux through reflux pump (07) pressurization after, send to
Overhead reflux；Residual acetic acid exports (051) output through acetic acid；Acetic acid for reflux adds before entering reactive distillation column (04)
Polymerization inhibitor, polymerization inhibitor is added to be provided by polymerization inhibitor tank (06), the polymerization inhibitor is 2,6-di-tert-butyl p-cresol, and boiling point is higher, energy
It is enough to be down to methacrylic anhydride tower reactor (042) from tower top；Meanwhile methacrylic anhydride tower reactor (042) is equipped with steam-heating system,
Minute quantity light substance enters tower top, the methacrylic anhydride that remaining purity is 96%, continuously from methyl-prop through rectification zone (043) again
Olefin(e) acid acid anhydride exports (046) output；Entire technique is finally set to tend towards stability.
After testing, the acetic acid purity for (051) output being exported by acetic acid is 99.3%；The conversion ratio of methacrylic acid is
99%, the yield of methacrylic anhydride is 90%.
Embodiment 2
(1) methacrylic acid is preheated in methacrylic acid entrance (014) into First Heat Exchanger (01), is led to after preheating
Control temperature control equipment (011) is crossed controlled at 90 DEG C, into reactive distillation column (04), is kept in reactive distillation column (04)
Vacuum degree -12KPa, methacrylic acid is interior by the interior negative pressure sucting reaction rectifying column (04) of reactive distillation column (04), and passes through mist
Change device (045) to be atomized；Acetic anhydride is preheated in acetic anhydride entrance (024) into the second heat exchanger (02) simultaneously, is preheated
Afterwards by controlling temperature control equipment (021) controlled at 90 DEG C, into reactive distillation column (04), acetic anhydride is by reacting essence
It evaporates in tower in negative pressure sucting reaction rectifying column (04), and be atomized by the atomizer (045) in tower, realizes methacrylic acid
Atomization with acetic anhydride contacts.
(2) feed rate that methacrylic acid is controlled by volume control device (012), passes through volume control device
(022) feed rate for controlling methacrylic acid, it is 2 to make the feed rate of the methacrylic acid and acetic anhydride ratio：1；It is described
Methacrylic acid and acetic anhydride are reacted in reaction zone (041), and the reaction zone (041) keeps anti-by steam-heating system
It answers temperature at 90 DEG C~100 DEG C, and keeps vacuum degree -12KPa；The low-boiling acetic acid crude product generated is reacted directly to described anti-
Rectification zone (043) on the upside of area (041) is answered to obtain acetic acid to top fractionation；The high boiling methacrylic anhydride warp that reaction generates
Rectification zone (043) obtains methacrylic anhydride and enters methacrylic anhydride tower reactor to bottom rectifying on the upside of the reaction zone (041)
(042)。
(3) after the acetic acid that step (2) obtains at the top of the reactive distillation column (04) by steaming, condensed device (03) cooling is cold
After solidifying, into return tank (05), control reflux ratio is 1：3, it after reflux pump (07) pressurization, will be sent to tower for the acetic acid of reflux
Top reflux；Residual acetic acid exports (051) output through acetic acid；Acetic acid for reflux is before entering reactive distillation column (04), addition
Polymerization inhibitor, polymerization inhibitor are provided by polymerization inhibitor tank (06), and the polymerization inhibitor is 2,6-di-tert-butyl p-cresol, and boiling point is higher, can
It is down to methacrylic anhydride tower reactor (042) from tower top；Meanwhile methacrylic anhydride tower reactor (042) is equipped with steam-heating system, pole
A small amount of light substance enters tower top, the methacrylic anhydride that remaining purity is 95%, continuously from metering system through rectification zone (043) again
Acid anhydrides exports (046) output；Entire technique is finally set to tend towards stability.
After testing, the acetic acid purity for (051) output being exported by acetic acid is 99.0%；The conversion ratio of methacrylic acid is
98%, the yield of methacrylic anhydride is 89%.
Embodiment 3
(1) methacrylic acid is preheated in methacrylic acid entrance (014) into First Heat Exchanger (01), is led to after preheating
Control temperature control equipment (011) is crossed controlled at 100 DEG C, into reactive distillation column (04), is protected in reactive distillation column (04)
Vacuum degree -10KPa is held, methacrylic acid is interior by the interior negative pressure sucting reaction rectifying column (04) of reactive distillation column (04), and passes through
Atomizer (045) is atomized；Acetic anhydride is preheated in acetic anhydride entrance (024) into the second heat exchanger (02) simultaneously, in advance
By controlling temperature control equipment (021) controlled at 80 DEG C after heat, into reactive distillation column (04), acetic anhydride passes through reaction
It in rectifying column in negative pressure sucting reaction rectifying column (04), and is atomized by the atomizer (045) in tower, realizes metering system
The atomization of acid and acetic anhydride contacts.
(2) feed rate that methacrylic acid is controlled by volume control device (012), passes through volume control device
(022) feed rate for controlling methacrylic acid, it is 2.8 to make the feed rate of the methacrylic acid and acetic anhydride ratio：1；Institute
It states methacrylic acid and acetic anhydride to be reacted in reaction zone (041), the reaction zone (041) is kept by steam-heating system
Reaction temperature keeps vacuum degree -10KPa at 90 DEG C~100 DEG C；The low-boiling acetic acid crude product generated is reacted directly to described
Rectification zone (043) obtains acetic acid to top fractionation on the upside of reaction zone (041)；React the high boiling methacrylic anhydride generated
It obtains methacrylic anhydride to bottom rectifying through rectification zone (043) on the upside of the reaction zone (041) and enters methacrylic anhydride tower
Kettle (042).
(3) after the acetic acid that step (2) obtains at the top of the reactive distillation column (04) by steaming, condensed device (03) cooling is cold
After solidifying, into return tank (05), control reflux ratio is 1：2, it after reflux pump (07) pressurization, will be sent to tower for the acetic acid of reflux
Top reflux；Residual acetic acid exports (051) output through acetic acid；Acetic acid for reflux is before entering reactive distillation column (04), addition
Polymerization inhibitor, polymerization inhibitor are provided by polymerization inhibitor tank (06), and the polymerization inhibitor is 2,6-di-tert-butyl p-cresol, and boiling point is higher, can
It is down to methacrylic anhydride tower reactor (042) from tower top；Meanwhile methacrylic anhydride tower reactor (042) is equipped with steam-heating system, pole
A small amount of light substance enters tower top, the methacrylic anhydride that remaining purity is 95%, continuously from metering system through rectification zone (043) again
Acid anhydrides exports (046) output；Entire technique is finally set to tend towards stability.
After testing, the acetic acid purity for (051) output being exported by acetic acid is 99.1%；The conversion ratio of methacrylic acid is
99%, the yield of methacrylic anhydride is 89.5%.
The above description of the disclosed embodiments enables professional and technical personnel in the field to realize or use this practicality new
Type.Various modifications to these embodiments will be apparent to those skilled in the art, and determine herein
The General Principle of justice can be realized in other embodiments without departing from the spirit or scope of the present utility model.Cause
This, the utility model is not intended to be limited to the embodiments shown herein, and is to fit to and principles disclosed herein
The widest range consistent with features of novelty.
Claims (10)
1. a kind of device of synthesizing methyl acrylic anhydride, including：
Reactive distillation column；The middle part of the reactive distillation column includes reaction zone and the rectifying positioned at the both sides up and down of the reaction zone
Area, tower top are equipped with acetic acid discharge port and filler entrance, and bottom of tower is equipped with methacrylic anhydride tower reactor；The reaction zone is equipped with methyl-prop
Olefin(e) acid feed inlet, acetic anhydride feed inlet and steam-heating system；
The First Heat Exchanger that discharge port is connected with the methacrylic acid feed inlet；
The second heat exchanger that discharge port is connected with the acetic anhydride feed inlet；
The condenser that feed inlet is connected with the acetic acid discharge port；The condenser is equipped with vacuum plant；
The return tank that feed inlet is connected with the discharge port of the condenser；The return tank is equipped with acetic acid outlet and reflux expects
Mouthful；Reflux material outlet is connected through reflux pump and return line with the filler entrance successively；
The polymerization inhibitor tank that discharge port is communicated with the return line.
2. the apparatus according to claim 1, which is characterized in that the methacrylic acid feed inlet is equipped with atomizer.
3. the apparatus according to claim 1, which is characterized in that the acetic anhydride feed inlet is equipped with atomizer.
4. the apparatus according to claim 1, which is characterized in that use filler in the rectification zone；The filler is regular
It is one or more in filler, Raschig ring and the poly- saddle ring of Pall ring.
5. the apparatus according to claim 1, which is characterized in that the methacrylic anhydride tower reactor is equipped with steam heating system
System, in-line analyzer and methacrylic anhydride outlet.
6. the apparatus according to claim 1, which is characterized in that the theoretical cam curve of the reactive distillation column is 10~35.
7. the apparatus according to claim 1, which is characterized in that the discharge port of the First Heat Exchanger is equipped with temperature control dress
It sets, volume control device and valve.
8. the apparatus according to claim 1, which is characterized in that the discharge port of second heat exchanger is equipped with temperature control dress
It sets, volume control device and valve.
9. the apparatus according to claim 1, which is characterized in that the condenser is equipped with in-line analyzer.
10. the apparatus according to claim 1, which is characterized in that the vacuum plant includes：
The vacuum tube communicated with the condenser；
The vacuum pump communicated with the vacuum tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201820125553.3U CN207987066U (en) | 2018-01-25 | 2018-01-25 | A kind of device of synthesizing methyl acrylic anhydride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201820125553.3U CN207987066U (en) | 2018-01-25 | 2018-01-25 | A kind of device of synthesizing methyl acrylic anhydride |
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| Publication Number | Publication Date |
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| CN207987066U true CN207987066U (en) | 2018-10-19 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201820125553.3U Withdrawn - After Issue CN207987066U (en) | 2018-01-25 | 2018-01-25 | A kind of device of synthesizing methyl acrylic anhydride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107963966A (en) * | 2018-01-25 | 2018-04-27 | 杭州和利时自动化有限公司 | A kind of device of synthesizing methyl acrylic anhydride |
-
2018
- 2018-01-25 CN CN201820125553.3U patent/CN207987066U/en not_active Withdrawn - After Issue
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107963966A (en) * | 2018-01-25 | 2018-04-27 | 杭州和利时自动化有限公司 | A kind of device of synthesizing methyl acrylic anhydride |
| CN107963966B (en) * | 2018-01-25 | 2023-11-21 | 杭州和利时自动化有限公司 | Device for synthesizing methacrylic anhydride |
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