CN104086405A - Apparatus for preparing butyric anhydride through reactive distillation of acetic anhydride and butyric acid, and process thereof - Google Patents
Apparatus for preparing butyric anhydride through reactive distillation of acetic anhydride and butyric acid, and process thereof Download PDFInfo
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- CN104086405A CN104086405A CN201410214054.8A CN201410214054A CN104086405A CN 104086405 A CN104086405 A CN 104086405A CN 201410214054 A CN201410214054 A CN 201410214054A CN 104086405 A CN104086405 A CN 104086405A
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- reactive distillation
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- butyric acid
- oxide
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- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 title claims abstract description 116
- YHASWHZGWUONAO-UHFFFAOYSA-N butanoyl butanoate Chemical compound CCCC(=O)OC(=O)CCC YHASWHZGWUONAO-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 238000000066 reactive distillation Methods 0.000 title claims abstract description 76
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 60
- 238000006243 chemical reaction Methods 0.000 claims abstract description 42
- 239000000463 material Substances 0.000 claims abstract description 13
- 230000000630 rising effect Effects 0.000 claims abstract description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 12
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 12
- 239000004571 lime Substances 0.000 claims description 12
- 238000012856 packing Methods 0.000 claims description 10
- 238000003672 processing method Methods 0.000 claims description 9
- 238000007599 discharging Methods 0.000 claims description 7
- AYNKGGWREYVHFZ-UHFFFAOYSA-N C(CCC)(=O)OC(CCC)=O.C(C)(=O)O Chemical compound C(CCC)(=O)OC(CCC)=O.C(C)(=O)O AYNKGGWREYVHFZ-UHFFFAOYSA-N 0.000 claims description 5
- -1 acetic acid acid anhydride Chemical class 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000007670 refining Methods 0.000 abstract 5
- BVQHHUQLZPXYAQ-UHFFFAOYSA-N acetyl butanoate Chemical compound CCCC(=O)OC(C)=O BVQHHUQLZPXYAQ-UHFFFAOYSA-N 0.000 abstract 1
- 238000010992 reflux Methods 0.000 abstract 1
- 239000000945 filler Substances 0.000 description 6
- 238000000605 extraction Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- DVECBJCOGJRVPX-UHFFFAOYSA-N butyryl chloride Chemical compound CCCC(Cl)=O DVECBJCOGJRVPX-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000010923 batch production Methods 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- GDIBTOVOAAOEMM-UHFFFAOYSA-N C(CCC)(=O)OC(CCC)=O.C(CCC)(=O)O Chemical compound C(CCC)(=O)OC(CCC)=O.C(CCC)(=O)O GDIBTOVOAAOEMM-UHFFFAOYSA-N 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- DZUDZSQDKOESQQ-UHFFFAOYSA-N cobalt hydrogen peroxide Chemical compound [Co].OO DZUDZSQDKOESQQ-UHFFFAOYSA-N 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- PXJJSXABGXMUSU-UHFFFAOYSA-N disulfur dichloride Chemical compound ClSSCl PXJJSXABGXMUSU-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- CCGKOQOJPYTBIH-UHFFFAOYSA-N ethenone Chemical compound C=C=O CCGKOQOJPYTBIH-UHFFFAOYSA-N 0.000 description 1
- MFBOGIVSZKQAPD-UHFFFAOYSA-M sodium butyrate Chemical compound [Na+].CCCC([O-])=O MFBOGIVSZKQAPD-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/54—Preparation of carboxylic acid anhydrides
- C07C51/56—Preparation of carboxylic acid anhydrides from organic acids, their salts, their esters or their halides, e.g. by carboxylation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses an apparatus for preparing butyric anhydride through reactive distillation of acetic anhydride and butyric acid, and a process thereof. The apparatus comprises a reactor, a reactive distillation tower, a butyric anhydride refining tower, a condenser, a condenser, a reboiler, a refluxing tank, a kettle tank, a pump and pipelines. The process using the combination of the reactive distillation tower, the rector and the butyric anhydride refining tower comprises the following steps: adding acetic anhydride and butyric acid to the reactor, reacting, and carrying out reaction and rectification on acetic anhydride and butyric acid flowing into the reactive distillation tower on each layer of trays of a reaction section; carrying out stripping section rectification on a material flowing down in the reaction section; carrying out rectifying section rectification on a material rising in the reactions section, and extracting from the tower top to obtain 80-100% acetic acid; pressurizing a material from the bottom of the reactive distillation tower to enter the butyric anhydride refining tower for rectification; and obtaining some of acetic acid, acetic anhydride, butyric acid, acetic butyric anhydride and butyric anhydride at the top of the butyric anhydride refining tower and butyric anhydride with the purity of 80-100% at the bottom of the refining tower. The apparatus and the process solve the problems of unstable quality, low yield and low production efficiency of products intermittently produced by using butyric anhydride.
Description
Technical field
The invention belongs to device and the processing method of butyryl oxide processed, particularly device and the processing method of a kind of diacetyl oxide and butyric acid reactive distillation butyryl oxide processed.
Technical background
Butyryl oxide conventional production methods has following several: butyryl chloride and Sodium propanecarboxylate be warm altogether, not easy-clear of the easy crystallization of this method by product sodium-chlor, and output is little, low conversion rate; Butyric acid does the catalyzer butyryl oxide that dewaters to obtain with sulfur subchloride, by product butyryl chloride contaminate environment, and side reaction is more; Butyric acid and ketene side reaction are more, and the purity of butyryl oxide is lower; Under cobalt dioxide catalysis, butyryl chloride and butyric acid can generate butyryl oxide in dichloromethane solvent, and productive rate is lower, and separating energy consumption is high; Diacetyl oxide and butyric acid exchange process, current domestic use interrupter method is produced, and the acetic acid constantly reaction being generated steams, and obtains the butyryl oxide that purity is higher, due to batch production, unstable product quality, yield is lower, and production efficiency is lower.
Summary of the invention
The object of the invention is to provide device and the processing method of a kind of diacetyl oxide and butyric acid reactive distillation butyryl oxide processed, utilizes the technical process of reactive distillation column association reaction device and butyryl oxide treating tower, can make diacetyl oxide and butyric acid butyryl oxide processed carry out continuously.
A kind of diacetyl oxide and butyric acid reactive distillation butyryl oxide device processed comprise: reactor 1, reactive distillation column 2, butyryl oxide treating tower 3, condenser 4,8, return tank 5,9, reboiler 6,10, reactor tank 7,11, the utility appliance such as pump 12-19 and pipeline.Reactive distillation column forms by 3 sections: rectifying section 20, conversion zone 21, stripping section 22.Butyryl oxide treating tower forms by 2 sections: rectifying section 23, stripping section 24.Pipeline comprises: pipeline 25-pipeline 54.
A kind of diacetyl oxide and butyric acid reactive distillation butyryl oxide device processed, is characterized in that: wherein there are the rectifying section (20), conversion zone (21), the stripping section (22) that connect up and down successively in reactive distillation column (2) inside; There are the rectifying section (23), the stripping section (24) that connect up and down successively in butyryl oxide treating tower (3) inside;
The upper lower nozzle of reactor (1) passes through respectively the upper lower nozzle of the conversion zone (23) of pump ligation rectifying tower, in reactor (1), side connects diacetyl oxide transfer lime through pump, and reactor (1) downside connects butyric acid transfer lime through pump;
Condenser (4) the lower-left end mouth of pipe before reactive distillation column (2) top push pipe mouth connects, return tank (5) the bottom mouth of pipe before the front condenser upper right side mouth of pipe connects, the front return tank upside mouth of pipe is through pump ligation rectifying tower top side pipe mouth, and the front return tank downside mouth of pipe connects acetic acid transfer lime; Reboiler (6) the upside mouth of pipe before the downside mouth of pipe of reactive distillation column connects, front reboiler bottom mouth of pipe ligation rectifier bottoms pipe and front reactor tank (7) the bottom mouth of pipe;
A mouth of pipe between the rectifying section (23) of front reactor tank side pipe mouth process pump connection butyryl oxide treating tower (3) and stripping section (24), the butyryl oxide treating tower top mouth of pipe connects aftercondenser (8) the lower-left end mouth of pipe, return tank (9) the bottom mouth of pipe after the aftercondenser upper right side mouth of pipe connects, the rear return tank upside mouth of pipe connects the butyryl oxide treating tower top side mouth of pipe through pump, and the rear return tank downside mouth of pipe connects ligation device (1) the upper side mouth of pipe through pump;
Reboiler (10) the upside mouth of pipe after the downside mouth of pipe of butyryl oxide treating tower connects, the rear reboiler bottom mouth of pipe connects butyryl oxide treating tower bottom tube and rear reactor tank (11) the bottom mouth of pipe, and rear reactor tank (11) the sidepiece mouth of pipe connects butyryl oxide transfer lime.
Described reactive distillation column rectifying section forms by 1 to 50 layer of column plate or by 1 to 10 meter of high packing section
Described reactive distillation column conversion zone forms by 5 to 50 layers of column plate or by 1 to 10 meter of high packing section
Described reactive distillation column stripping section forms by 1 to 50 layer of column plate or by 1 to 10 meter of high packing section
Described butyryl oxide treating tower rectifying section forms by 1-50 layer column plate or by 1 to 10 meter of high packing section
Described butyryl oxide treating tower stripping section forms by 1-50 layer column plate or by 1 to 10 meter of high packing section
Described reactor can be 1 to 10 parallel operation.
The processing method step that adopts diacetyl oxide and butyric acid reactive distillation butyryl oxide device processed to carry out diacetyl oxide and butyric acid reactive distillation butyryl oxide processed is:
1) diacetyl oxide and butyric acid enter after reactor reaction, from reactor top or bottom, enter certain several position of reactive distillation column rectifying section bottom to conversion zone bottom by pipeline;
2) enter diacetyl oxide and the butyric acid of reactive distillation column, on every layer of column plate of conversion zone, react and rectifying simultaneously;
3) material flowing down through conversion zone is through the rectifying of reactive distillation column stripping section;
4) material rising through conversion zone is through the rectifying of reactive distillation column rectifying section, and overhead product obtains acetic acid through condenser condenses;
5) discharging of reactive distillation column tower reactor enters the rectifying of butyric acid treating tower by pump pressurization;
6) butyric acid treating tower tower top obtains certain several material in acetic acid, butyric acid, diacetyl oxide, acetic acid butyryl oxide, butyryl oxide, and overhead product is returned reactor by pump through pipeline and continued reaction after condenser condenses;
7) butyric acid treating tower tower reactor obtains high purity butylene acid anhydrides.
In this technical process, raw acetic acid acid anhydride and butyric acid mol ratio are 1:10～5:1.
In this technical process, the working pressure of reactive distillation column is being 5～200kPa (absolute pressure), and the working pressure of butyryl oxide treating tower is 5～500kPa (absolute pressure).
Beneficial effect of the present invention:
Utilize the technical process of reactive distillation column association reaction device and butyryl oxide treating tower, can make diacetyl oxide and butyric acid reactive distillation butyryl oxide processed carry out continuously, by butyryl oxide treating tower tower reactor discharging butyryl oxide content 80～100%, reactive distillation column ejects material acetic acid content 80-100%.Butyryl oxide batch production unstable product quality, yield is lower, production efficiency is lower problem are solved.
Brief description of the drawings
Fig. 1 is the device schematic diagram of diacetyl oxide and butyric acid reactive distillation butyryl oxide processed.
In figure: 1 reactor, 2 reactive distillation columns, 3 butyryl oxide treating towers, 4 front condensers, 5 front return tanks, 6 front reboilers, 7 front reactor tanks, 8 aftercondensers, 9 rear return tanks, 10 rear reboilers, 11 rear reactor tanks, 12-19 pump, 20 rectifying sections, 21 conversion zones, 22 stripping sections, 23 rectifying sections, 24 stripping sections, 25-54 pipeline.
Embodiment
As shown in Figure 1, a kind of diacetyl oxide and butyric acid reactive distillation butyryl oxide device processed, wherein there are the rectifying section (20), conversion zone (21), the stripping section (22) that connect up and down successively in reactive distillation column (2) inside; There are the rectifying section (23), the stripping section (24) that connect up and down successively in butyryl oxide treating tower (3) inside;
The upper lower nozzle of reactor (1) passes through respectively the upper lower nozzle of the conversion zone (23) of pump ligation rectifying tower, in reactor (1), side connects diacetyl oxide transfer lime through pump, and reactor (1) downside connects butyric acid transfer lime through pump;
Condenser (4) the lower-left end mouth of pipe before reactive distillation column (2) top push pipe mouth connects, return tank (5) the bottom mouth of pipe before the front condenser upper right side mouth of pipe connects, the front return tank upside mouth of pipe is through pump ligation rectifying tower top side pipe mouth, and the front return tank downside mouth of pipe connects acetic acid transfer lime; Reboiler (6) the upside mouth of pipe before the downside mouth of pipe of reactive distillation column connects, front reboiler bottom mouth of pipe ligation rectifier bottoms pipe and front reactor tank (7) the bottom mouth of pipe;
A mouth of pipe between the rectifying section (23) of front reactor tank side pipe mouth process pump connection butyryl oxide treating tower (3) and stripping section (24), the butyryl oxide treating tower top mouth of pipe connects aftercondenser (8) the lower-left end mouth of pipe, return tank (9) the bottom mouth of pipe after the aftercondenser upper right side mouth of pipe connects, the rear return tank upside mouth of pipe connects the butyryl oxide treating tower top side mouth of pipe through pump, and the rear return tank downside mouth of pipe connects ligation device (1) the upper side mouth of pipe through pump;
Reboiler (10) the upside mouth of pipe after the downside mouth of pipe of butyryl oxide treating tower connects, the rear reboiler bottom mouth of pipe connects butyryl oxide treating tower bottom tube and rear reactor tank (11) the bottom mouth of pipe, and rear reactor tank (11) the sidepiece mouth of pipe connects butyryl oxide transfer lime.
Reactive distillation column rectifying section in the present invention is made up of 1 to 30 layer of column plate, also can be by the various media assemblages of certain altitude.
Reactive distillation column conversion zone in the present invention is made up of 5 to 50 layers of column plate, also can be by the various media assemblages of certain altitude.
Reactive distillation column stripping section in the present invention is made up of 1 to 30 layer of column plate, also can be by the various media assemblages of certain altitude.
Butyryl oxide treating tower rectifying section in the present invention is made up of 1-30 layer column plate, also can be by the various media assemblages of certain altitude.
Butyryl oxide treating tower stripping section in the present invention is made up of 1-30 layer column plate, also can be by the various media assemblages of certain altitude.
Reactor in the present invention can be 1 to 10 parallel operation.
Raw acetic acid acid anhydride in the present invention and butyric acid mol ratio are 1:10～5:1.
The processing method step that adopts diacetyl oxide of the present invention and butyric acid reactive distillation butyryl oxide device processed to carry out diacetyl oxide and butyric acid reactive distillation butyryl oxide processed is:
Diacetyl oxide is thrown reactor reaction into by pump 12, pump 13 from pipeline 25, butyric acid respectively from pipeline 26.After reaction, discharging is thrown certain position between reactive distillation column 2 rectifying section 20 bottoms and conversion zone 21 bottoms into by pump 14, pump 15 respectively by pipeline 29, pipeline 31.The unreacted diacetyl oxide of material that enters this tower reacts on these conversion zone 21 every layer of column plates with butyric acid, simultaneously diacetyl oxide, butyric acid and react the acetic acid, acetic acid butyryl oxide, the butyryl oxide rectifying on every layer of column plate of this tower that generate afterwards.The acetic acid that reaction generates, by overhead extraction, enters condenser 4 through pipeline 33.After condensation, liquid enters return tank 5 via pipeline 34.Acetic acid by pipeline 36 from return tank extraction purity 80%-100%.Part acetic acid via pump 16 is back to reactive distillation column overhead.Certain several material in acetic acid, acetic acid butyryl oxide, butyryl oxide that unreacted diacetyl oxide and butyric acid or reaction generate, via tower reactor extraction, enter reactor tank 7 by pipeline 40.Liquid in reactor tank 7 is thrown butyryl oxide treating tower 3 into via pump 17 and is refined.Butyryl oxide treating tower 3 tower tops are given vent to anger and are made up of certain several material in acetic acid, diacetyl oxide, butyric acid, acetic acid butyryl oxide, butyryl oxide, enter condenser 8 through pipeline 49, and condensation enters return tank 9 via pipeline 49.In return tank 9, liquid portion is back to butyryl oxide treating tower tower top via pump 18, and partially liq is returned reactor 1 via pump 19 and continued reaction.Butyryl oxide treating tower 3 tower reactors are via reactor tank 11, can extraction high purity butylene acid anhydrides, and butyryl oxide content is 80%～100%.
The working pressure of the reactive distillation column in the present invention is being 5～100kPa (absolute pressure), and the working pressure of butyryl oxide treating tower is 5～500kPa (absolute pressure).
Application example 1
Reactive distillation column is made up of 3 parts: 5 meters of fillers of rectifying section (reactive distillation filler), 30 layers of column plate of conversion zone (Reactive Stage), 13 layers of column plate of stripping section (Reactive Stage), 1.2 meters of tower diameters.8 layers of column plate of diacetyl oxide treating tower rectifying section, 4 meters of fillers of stripping section, 0.8 meter of tower diameter.Diacetyl oxide and butyric acid raw materials components mole ratio are 0.33,0.5,1, reactive distillation column working pressure is 10kPa (absolute pressure), butyryl oxide treating tower working pressure 1atm (absolute pressure), butyryl oxide treating tower tower reactor discharging butyryl oxide purity 95.4%, 93.8%, 84.7%.
Application example 2
Reactive distillation column is made up of 3 parts: 10 layers of column plate of rectifying section (Reactive Stage), 25 layers of column plate of conversion zone (Reactive Stage), 3 meters of fillers of stripping section (reactive distillation filler), 1.5 meters of tower diameters.3 meters of fillers of diacetyl oxide treating tower rectifying section, 12 layers of column plate of stripping section, 1 meter of tower diameter.Diacetyl oxide and butyric acid raw materials components mole ratio are 1,2,3, reactive distillation column working pressure is 20kPa (absolute pressure), butyryl oxide treating tower working pressure 1.1atm (absolute pressure), butyryl oxide treating tower tower reactor discharging butyryl oxide purity 92.1%, 83.5%, 62.3%.
Reaction example 3
Reactive distillation column is made up of 3 parts: 12 layers of column plate of rectifying section (Reactive Stage), 28 layers of column plate of conversion zone (Reactive Stage), 15 layers of column plate of stripping section (Reactive Stage), 1 meter of tower diameter.10 layers of column plate of diacetyl oxide treating tower rectifying section, 10 layers of column plate of stripping section, 0.6 meter of tower top.Diacetyl oxide and butyric acid raw materials components mole ratio are 0.5, reactive distillation column working pressure is 35kPa (absolute pressure), 25kPa (absolute pressure), 15kPa (absolute pressure), butyryl oxide treating tower working pressure is 1atm (absolute pressure), and in the discharging of butyryl oxide treating tower tower reactor, butyryl oxide purity is 89.4%, 93.5%, 96.7%.
Claims (10)
1. a diacetyl oxide and butyric acid reactive distillation butyryl oxide device processed, is characterized in that: wherein there are the rectifying section (20), conversion zone (21), the stripping section (22) that connect up and down successively in reactive distillation column (2) inside; There are the rectifying section (23), the stripping section (24) that connect up and down successively in butyryl oxide treating tower (3) inside;
The upper lower nozzle of reactor (1) passes through respectively the upper lower nozzle of the conversion zone (23) of pump ligation rectifying tower, in reactor (1), side connects diacetyl oxide transfer lime through pump, and reactor (1) downside connects butyric acid transfer lime through pump;
Condenser (4) the lower-left end mouth of pipe before reactive distillation column (2) top push pipe mouth connects, return tank (5) the bottom mouth of pipe before the front condenser upper right side mouth of pipe connects, the front return tank upside mouth of pipe is through pump ligation rectifying tower top side pipe mouth, and the front return tank downside mouth of pipe connects acetic acid transfer lime; Reboiler (6) the upside mouth of pipe before the downside mouth of pipe of reactive distillation column connects, front reboiler bottom mouth of pipe ligation rectifier bottoms pipe and front reactor tank (7) the bottom mouth of pipe;
A mouth of pipe between the rectifying section (23) of front reactor tank side pipe mouth process pump connection butyryl oxide treating tower (3) and stripping section (24), the butyryl oxide treating tower top mouth of pipe connects aftercondenser (8) the lower-left end mouth of pipe, return tank (9) the bottom mouth of pipe after the aftercondenser upper right side mouth of pipe connects, the rear return tank upside mouth of pipe connects the butyryl oxide treating tower top side mouth of pipe through pump, and the rear return tank downside mouth of pipe connects ligation device (1) the upper side mouth of pipe through pump;
Reboiler (10) the upside mouth of pipe after the downside mouth of pipe of butyryl oxide treating tower connects, the rear reboiler bottom mouth of pipe connects butyryl oxide treating tower bottom tube and rear reactor tank (11) the bottom mouth of pipe, and rear reactor tank (11) the sidepiece mouth of pipe connects butyryl oxide transfer lime.
2. diacetyl oxide according to claim 1 and butyric acid reactive distillation butyryl oxide device processed, is characterized in that: described reactive distillation column rectifying section forms by 1 to 50 layer of column plate or by 1 to 10 meter of high packing section.
3. diacetyl oxide according to claim 1 and butyric acid reactive distillation butyryl oxide device processed, is characterized in that: described reactive distillation column conversion zone forms by 5 to 50 layers of column plate or by 1 to 10 meter of high packing section.
4. diacetyl oxide according to claim 1 and butyric acid reactive distillation butyryl oxide device processed, is characterized in that: described reactive distillation column stripping section forms by 1 to 50 layer of column plate or by 1 to 10 meter of high packing section.
5. diacetyl oxide according to claim 1 and butyric acid reactive distillation butyryl oxide device processed, is characterized in that: described butyryl oxide treating tower rectifying section forms by 1-50 layer column plate or by 1 to 10 meter of high packing section.
6. diacetyl oxide according to claim 1 and butyric acid reactive distillation butyryl oxide device processed, is characterized in that: described butyryl oxide treating tower stripping section forms by 1-50 layer column plate or by 1 to 10 meter of high packing section.
7. diacetyl oxide according to claim 1 and butyric acid reactive distillation butyryl oxide device processed, is characterized in that: described reactor is 1 to 10 parallel operation.
8. a processing method for diacetyl oxide and butyric acid reactive distillation butyryl oxide processed, is characterized in that: employing diacetyl oxide and butyric acid reactive distillation butyryl oxide device processed carry out it step comprising and be:
1) diacetyl oxide and butyric acid enter after reactor reaction, from reactor top or bottom, enter certain several position of reactive distillation column rectifying section bottom to conversion zone bottom by pipeline;
2) enter diacetyl oxide and the butyric acid of reactive distillation column, on every layer of column plate of conversion zone, react and rectifying simultaneously;
3) material flowing down through conversion zone is through the rectifying of reactive distillation column stripping section;
4) material rising through conversion zone is through the rectifying of reactive distillation column rectifying section, and overhead product obtains the mixture of acetic acid or acetic acid and butyric acid, diacetyl oxide through condenser condenses.
5) discharging of reactive distillation column tower reactor enters the rectifying of butyryl oxide treating tower by pump pressurization;
6) butyric acid treating tower tower top obtains certain several material in acetic acid, butyric acid, diacetyl oxide, acetic acid butyryl oxide, butyryl oxide, and overhead product is returned reactor by pump through pipeline and continued reaction after condenser condenses;
7) butyric acid treating tower tower reactor obtains butyryl oxide.
9. the processing method of diacetyl oxide according to claim 8 and butyric acid reactive distillation butyryl oxide processed, is characterized in that: the mol ratio of raw acetic acid acid anhydride and butyric acid is 1:10～5:1.
10. the processing method of diacetyl oxide according to claim 8 and butyric acid reactive distillation butyryl oxide processed, is characterized in that: the operation absolute pressure pressure of reactive distillation column is 5～200kPa, and the operation absolute pressure pressure of butyryl oxide treating tower is 5～500kPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410214054.8A CN104086405A (en) | 2014-05-21 | 2014-05-21 | Apparatus for preparing butyric anhydride through reactive distillation of acetic anhydride and butyric acid, and process thereof |
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| CN201410214054.8A CN104086405A (en) | 2014-05-21 | 2014-05-21 | Apparatus for preparing butyric anhydride through reactive distillation of acetic anhydride and butyric acid, and process thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112047834A (en) * | 2020-08-11 | 2020-12-08 | 浙江恒澜科技有限公司 | Device and method for continuously preparing isobutyric anhydride |
| CN114805057A (en) * | 2022-06-10 | 2022-07-29 | 福建技术师范学院 | Production method for producing butyric anhydride by bulkhead reaction and rectification |
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| JP4014954B2 (en) * | 2002-07-08 | 2007-11-28 | 株式会社トクヤマ | Method for producing acrylic anhydride or methacrylic anhydride |
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2014
- 2014-05-21 CN CN201410214054.8A patent/CN104086405A/en active Pending
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|---|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112047834A (en) * | 2020-08-11 | 2020-12-08 | 浙江恒澜科技有限公司 | Device and method for continuously preparing isobutyric anhydride |
| CN114805057A (en) * | 2022-06-10 | 2022-07-29 | 福建技术师范学院 | Production method for producing butyric anhydride by bulkhead reaction and rectification |
| CN114805057B (en) * | 2022-06-10 | 2024-02-02 | 福建技术师范学院 | A production method for producing butyric anhydride by bulkhead reaction distillation |
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