CN115260034A - Original start-up and stop method for producing ethyl acetate by using industrial ionic liquid catalyst - Google Patents
Original start-up and stop method for producing ethyl acetate by using industrial ionic liquid catalyst Download PDFInfo
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- CN115260034A CN115260034A CN202111516411.2A CN202111516411A CN115260034A CN 115260034 A CN115260034 A CN 115260034A CN 202111516411 A CN202111516411 A CN 202111516411A CN 115260034 A CN115260034 A CN 115260034A
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- 239000002608 ionic liquid Substances 0.000 title claims abstract description 124
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 239000003054 catalyst Substances 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 207
- 230000008929 regeneration Effects 0.000 claims abstract description 81
- 238000011069 regeneration method Methods 0.000 claims abstract description 81
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 61
- 238000011084 recovery Methods 0.000 claims abstract description 55
- 238000000066 reactive distillation Methods 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 238000012432 intermediate storage Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims description 15
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 12
- 238000005070 sampling Methods 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 claims description 8
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 8
- -1 alkyl pyridine hydrogen sulfate Chemical compound 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 6
- 238000004364 calculation method Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- 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
Abstract
The invention discloses an original start-up and stop method for producing ethyl acetate by an industrialized ionic liquid catalyst. Controlling the acetic acid recovery tower to start to feed ethanol through a valve, simultaneously discharging materials to the acetic acid recovery tower from the bottom of the reactive distillation tower, controlling the reaction and recovery regeneration units well, completing the start-up, finally stopping the heating of the reboiler and the transportation of all pumps, controlling the liquid levels of the reactive distillation tower, the acetic acid recovery tower, the intermediate storage tank and the ionic liquid regeneration kettle well, and waiting for the start-up again next time; according to the invention, through a series of valve control, the problems of pipeline blockage and pump transportation caused by the fact that the viscosity of the ionic liquid is increased due to too high concentration can be effectively avoided; the method is an effective industrialized solution, and has the advantages of advanced process, simple operation, stable and reliable effect and the like.
Description
Technical Field
The invention relates to a series of treatment methods for reactive extraction, rectification and regeneration, in particular to an original starting and stopping method for producing ethyl acetate by using an industrial ionic liquid catalyst.
Background
The production of ethyl acetate by using the ionic liquid as the catalyst is mature in laboratory level, but most of the prior art is single-pass test, and the difficulty of application of the characteristics of the ionic liquid in an industrial process is not studied. In the process of starting and stopping, the problems of pipeline blockage and pump transportation caused by overhigh concentration and large viscosity of the ionic liquid are solved, and a proper solution scheme is not found in the prior art.
Disclosure of Invention
Aiming at the problems, the invention aims to provide an original start-stop method for producing ethyl acetate by using an industrial ionic liquid catalyst, which solves the problems of pipeline blockage and pump transportation caused by overhigh concentration and increased viscosity of the ionic liquid in the start-stop process of producing ethyl acetate by using the industrial ionic liquid catalyst.
In order to realize the purpose of the invention, the invention is realized by the following technical scheme: an original start-up and shut-down method for producing ethyl acetate by using an industrial ionic liquid catalyst comprises the following steps:
the method comprises the following steps: firstly, preparing an aqueous solution with the ionic liquid content of sixty percent to eighty percent in advance, transferring the aqueous solution to an ionic liquid regeneration kettle, and transferring the ionic liquid aqueous solution in the regeneration kettle to a reaction rectifying tower through a pump until the liquid level of the tower bottom reaches twenty percent to fifty percent;
step two: through valve control, the ionic liquid aqueous solution reaches the acetic acid recovery tower through the ionic liquid regeneration kettle, then reaches the intermediate storage tank from the acetic acid recovery tower, and returns to the ionic liquid regeneration kettle for circulation, then the regeneration function of the ionic liquid regeneration kettle is started for regeneration, and sampling is carried out at the bottom of the ionic liquid regeneration kettle every fifteen to thirty minutes to analyze the content of the ionic liquid;
step three: starting a reaction rectifying tower reboiler to heat the reaction rectifying tower, and sampling and analyzing the bottom of the ionic liquid regeneration kettle when the temperature of the top of the reaction rectifying tower reaches the boiling point of ethyl acetate until the temperature is qualified;
step four: firstly, acetic acid is fed into a reactive distillation tower according to a specific flow, after a specific time, the reactive distillation tower starts to feed an analytically qualified ionic liquid catalyst through the switching of a valve, and then ethanol is fed into the reactive distillation tower through a certain time;
step five: after fifty percent of liquid level exists at the bottom of the reactive distillation tower, controlling the acetic acid recovery tower to start to feed ethanol through a valve, simultaneously discharging materials to the acetic acid recovery tower from the bottom of the reactive distillation tower, controlling a reaction and recovery regeneration unit well, and finishing the start-up;
step six: when the vehicle is ready to stop, firstly, the regeneration function of the ionic liquid regeneration kettle is closed, then the feeding of ethanol and acetic acid of the reaction rectifying tower is cut off, the water-containing ionic liquid catalyst in the ionic liquid regeneration kettle is pumped into the acetic acid recovery tower through the control of a valve, the feeding of ethanol in the acetic acid recovery tower is stopped, and finally, the feeding of the ionic liquid in the reaction rectifying tower is cut off;
step seven: and finally, stopping the heating of the reboiler and the transportation of all pumps, well controlling the liquid levels of the reaction rectifying tower, the acetic acid recovery tower, the intermediate storage tank and the ionic liquid regeneration kettle, and waiting for the next start-up.
The further improvement is that: the reaction rectifying tower is connected with the ionic liquid regeneration kettle through a pipeline, a pipeline flange is connected with a first valve, the reaction rectifying tower is connected with an acetic acid recovery tower through a pipeline, the pipeline flange is connected with a second valve, the acetic acid recovery tower is connected with the ionic liquid regeneration kettle through a pipeline, the pipeline flange is connected with a fifth valve, the ethanol feeding device is respectively connected with the reaction rectifying tower and the acetic acid recovery tower through pipelines, and the pipelines are respectively connected with a fourth valve and a third valve. The acetic acid recovery tower is connected with an intermediate storage tank through a pipeline, and the intermediate storage tank is connected with the ionic liquid regeneration kettle through a pipeline.
The further improvement is that: in the second step, the valve is controlled by the valve, the state of the valve is that the fifth valve is opened, the first valve to the fourth valve are closed, and the ionic liquid content is sampled and analyzed at the bottom of the ionic liquid regeneration kettle at intervals, wherein the time can depend on the regeneration capacity of the regeneration kettle and is fifteen to thirty minutes.
The further improvement is that: in the third step, the boiling point of the ethyl acetate is seventy-seven ℃, and the ionic liquid content analyzed at the bottom of the ionic liquid regeneration kettle is higher than ninety-five percent, so that the product is qualified.
The further improvement lies in that: in the fourth step, the time obtained by calculation according to the internal design of the reactive distillation column and the distance between the acetic acid feed port and the ionic liquid feed port is obtained after the specific time, the valves are switched, the first valve, the fourth valve and the fifth valve are opened, the second valve and the third valve are closed, and finally the time is obtained by calculation according to the internal design of the reactive distillation column and the distance between the ethanol feed port and the ionic liquid feed port after the specific time.
The further improvement lies in that: and a liquid level is arranged at the bottom of the reaction rectifying tower in the step five, the liquid level ranges from forty percent to seventy percent, the acetic acid recovery tower is controlled by a valve to start to feed ethanol, the bottom of the reaction rectifying tower starts to discharge materials to the acetic acid recovery tower, and the valves are in open states from the first valve to the fifth valve.
The further improvement lies in that: and in the sixth step, the feed of the ethanol and the acetic acid in the reactive distillation column is cut off, namely the fourth valve is closed, the acetic acid feed valve is closed, the second valve, the third valve and the fourth valve are closed through valve control, the first valve and the fifth valve are opened, and finally the feed of the water-containing ionic liquid in the reactive distillation column and the acetic acid recovery column is cut off, namely the first valve and the fifth valve are closed.
The further improvement lies in that: the ionic liquid is a mixture of seven components of pyridine, alkyl pyridine hydrogen sulfate and hydrogen phosphate, imidazole, alkyl imidazole hydrogen sulfate and hydrogen phosphate and free acid, and is a catalyst for catalyzing acidic substances and alcohol substances to react to produce ester substances.
The invention has the beneficial effects that: the invention can effectively avoid the problems of pipeline blockage and pump transportation caused by the fact that the viscosity of the ionic liquid is increased due to overhigh concentration through the control of a series of valves. The method is an effective industrialized solution, and has the advantages of advanced process, simple operation, stable and reliable effect and the like.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
In order to further understand the present invention, the following detailed description will be made with reference to the following examples, which are only used for explaining the present invention and are not to be construed as limiting the scope of the present invention.
Example one
According to the illustration in fig. 1, this embodiment provides an original start-up and shut-down method for producing ethyl acetate by using an industrial ionic liquid catalyst, comprising the following steps:
the method comprises the following steps: firstly, preparing an aqueous solution with the ionic liquid content of sixty percent to eighty percent in advance, transferring the aqueous solution to an ionic liquid regeneration kettle, and transferring the ionic liquid aqueous solution in the regeneration kettle to a reaction rectifying tower through a pump until the liquid level of the tower bottom reaches twenty percent to fifty percent;
step two: through valve control, the ionic liquid aqueous solution reaches the acetic acid recovery tower through the ionic liquid regeneration kettle, then reaches the intermediate storage tank from the acetic acid recovery tower, and returns to the ionic liquid regeneration kettle for circulation, then the regeneration function of the ionic liquid regeneration kettle is started for regeneration, and sampling is carried out at the bottom of the ionic liquid regeneration kettle every fifteen to thirty minutes to analyze the content of the ionic liquid;
step three: starting a reaction rectifying tower reboiler to heat the reaction rectifying tower, and sampling and analyzing the bottom of the ionic liquid regeneration kettle until the temperature of the top of the reaction rectifying tower reaches the boiling point of ethyl acetate until the ionic liquid regeneration kettle is qualified;
step four: firstly, acetic acid is fed into a reactive distillation tower according to a specific flow, after a specific time, the reactive distillation tower starts to feed an analytically qualified ionic liquid catalyst through the switching of a valve, and then ethanol is fed into the reactive distillation tower through a certain time;
step five: after fifty percent of liquid level exists at the bottom of the reactive distillation tower, controlling the acetic acid recovery tower to start to feed ethanol through a valve, simultaneously discharging materials to the acetic acid recovery tower from the bottom of the reactive distillation tower, controlling a reaction and recovery regeneration unit well, and finishing the start-up;
step six: when the vehicle is ready to stop, firstly, the regeneration function of the ionic liquid regeneration kettle is closed, then the feeding of ethanol and acetic acid of the reaction rectifying tower is cut off, the water-containing ionic liquid catalyst in the ionic liquid regeneration kettle is pumped into the acetic acid recovery tower through the control of a valve, the feeding of ethanol in the acetic acid recovery tower is stopped, and finally, the feeding of the ionic liquid in the reaction rectifying tower is cut off;
step seven: and finally, stopping the heating of the reboiler and the transportation of all pumps, well controlling the liquid levels of the reaction rectifying tower, the acetic acid recovery tower, the intermediate storage tank and the ionic liquid regeneration kettle, and waiting for the next start-up.
The reaction rectifying tower is connected with the ionic liquid regeneration kettle through a pipeline, a pipeline flange is connected with a first valve, the reaction rectifying tower is connected with an acetic acid recovery tower through a pipeline, the pipeline flange is connected with a second valve, the acetic acid recovery tower is connected with the ionic liquid regeneration kettle through a pipeline, the pipeline flange is connected with a fifth valve, the ethanol feeding device is respectively connected with the reaction rectifying tower and the acetic acid recovery tower through pipelines, and the pipelines are respectively connected with a fourth valve and a third valve. The acetic acid recovery tower is connected with an intermediate storage tank through a pipeline, and the intermediate storage tank is connected with the ionic liquid regeneration kettle through a pipeline.
In the second step, the valve is controlled by the valve, the state of the valve is that the fifth valve is opened, the first valve to the fourth valve are closed, and the ionic liquid content is sampled and analyzed at the bottom of the ionic liquid regeneration kettle at intervals, wherein the time can depend on the regeneration capacity of the regeneration kettle and is fifteen to thirty minutes.
In the third step, the boiling point of the ethyl acetate is seventy-seven ℃, and the ionic liquid content analyzed at the bottom of the ionic liquid regeneration kettle is more than ninety-five percent, so that the product is qualified.
In the fourth step, the time obtained by calculation according to the internal design of the reactive distillation column and the distance between the acetic acid feed port and the ionic liquid feed port is obtained after the specific time, the valves are switched, the first valve, the fourth valve and the fifth valve are opened, the second valve and the third valve are closed, and finally the time is obtained by calculation according to the internal design of the reactive distillation column and the distance between the ethanol feed port and the ionic liquid feed port.
And a liquid level is arranged at the bottom of the reaction rectifying tower in the step five, the liquid level ranges from forty percent to seventy percent, the acetic acid recovery tower is controlled by a valve to start to feed ethanol, the bottom of the reaction rectifying tower starts to discharge materials to the acetic acid recovery tower, and the valves are in open states from the first valve to the fifth valve.
In the sixth step, the feeding of the ethanol and the acetic acid in the reactive distillation column is cut off, namely the fourth valve is closed, the acetic acid feeding valve is closed, the second valve, the third valve and the fourth valve are closed through valve control, the first valve and the fifth valve are opened, and finally the feeding of the water-containing ionic liquid in the reactive distillation column and the acetic acid recovery column is cut off, namely the first valve and the fifth valve are closed.
The ionic liquid is a mixture of seven components of pyridine, alkyl pyridine hydrogen sulfate and hydrogen phosphate, imidazole, alkyl imidazole hydrogen sulfate and hydrogen phosphate and free acid, and is a catalyst for catalyzing acidic substances and alcohol substances to react to produce ester substances.
When the ionic liquid is used, the ionic liquid is prepared by mixing seven components of pyridine, alkyl pyridine hydrogen sulfate and hydrogen phosphate, imidazole, alkyl imidazole hydrogen sulfate and hydrogen phosphate, free acid and the like, the ionic liquid is a catalyst for catalyzing the reaction of acetic acid and ethanol to produce ethyl acetate, aqueous solution with eighty percent of ionic liquid content is prepared and transferred to an ionic liquid regeneration kettle, and the ionic liquid aqueous solution in the regeneration kettle is transferred to a reaction rectifying tower through a pump until the liquid level reaches twenty percent; opening a fifth valve to enable the ionic liquid aqueous solution to pass through an ionic liquid regeneration kettle, an acetic acid recovery tower, an intermediate storage tank and then return to the ionic liquid regeneration kettle for circulation, opening the regeneration function of the ionic liquid regeneration kettle for regeneration, sampling and analyzing at the bottom of the ionic liquid regeneration kettle every twenty minutes, then simultaneously opening a reboiler of the reactive distillation tower to heat the reactive distillation tower, and when the temperature of the top of the reactive distillation tower reaches seventy-seven ℃, sampling and analyzing at the bottom of the ionic liquid regeneration kettle to enable the ionic liquid content to be ninety-six percent according to 10m3Firstly, acetic acid is fed into a reaction rectifying tower, a first valve is opened after five minutes, the reaction rectifying tower is fed with an ionic liquid catalyst qualified by analysis, a fourth valve is opened after three minutes to enable the reaction rectifying tower to start feeding ethanol, then a third valve is opened to control an acetic acid recovery tower to start feeding ethanol after fifty percent of liquid level exists at the bottom of the reaction rectifying tower, a second valve is opened to enable the bottom of the reaction rectifying tower to start discharging to the acetic acid recovery tower, reaction is controlled, a recovery and regeneration unit is started, finally, when parking is prepared, firstly, the feeding of ethanol and acetic acid of the reaction rectifying tower is cut off by closing the fourth valve and the acetic acid feeding valve, the regeneration function of an ionic liquid regeneration kettle is closed, and a water-containing ionic liquid in the ionic liquid regeneration kettle is regenerated by closing the second valve and the third valveAnd pumping the bulk catalyst into the reaction rectifying tower and the acetic acid recovery tower, closing the first valve and the fifth valve, stopping the heating of the reboiler and the transportation of all pumps, controlling the liquid levels of the reaction rectifying tower, the acetic acid recovery tower, the intermediate storage tank and the ionic liquid regeneration kettle, and starting the reactor again for the next time, so that the original starting and stopping method for producing ethyl acetate by using the industrial ionic liquid catalyst is completed.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. An original start-up and shut-down method for producing ethyl acetate by using an industrial ionic liquid catalyst is characterized by comprising the following steps of:
the method comprises the following steps: firstly, preparing an aqueous solution with the ionic liquid content of sixty percent to eighty percent in advance, transferring the aqueous solution to an ionic liquid regeneration kettle, and transferring the ionic liquid aqueous solution in the regeneration kettle to a reaction rectifying tower through a pump until the liquid level of the tower bottom reaches twenty percent to fifty percent;
step two: through valve control, the ionic liquid aqueous solution reaches the acetic acid recovery tower through the ionic liquid regeneration kettle, then reaches the intermediate storage tank from the acetic acid recovery tower, and returns to the ionic liquid regeneration kettle for circulation, then the regeneration function of the ionic liquid regeneration kettle is started for regeneration, and sampling is carried out at the bottom of the ionic liquid regeneration kettle every fifteen to thirty minutes to analyze the content of the ionic liquid;
step three: starting a reaction rectifying tower reboiler to heat the reaction rectifying tower, and sampling and analyzing the bottom of the ionic liquid regeneration kettle when the temperature of the top of the reaction rectifying tower reaches the boiling point of ethyl acetate until the temperature is qualified;
step four: firstly, acetic acid is fed into a reactive distillation tower according to a specific flow, after a specific time, the reactive distillation tower starts to feed an analytically qualified ionic liquid catalyst through the switching of a valve, and then ethanol is fed into the reactive distillation tower through a certain time;
step five: after fifty percent of liquid level exists at the bottom of the reaction rectifying tower, controlling the acetic acid recovery tower to start to feed ethanol through a valve, simultaneously, controlling the bottom of the reaction rectifying tower to discharge to the acetic acid recovery tower, controlling a reaction and recovery regeneration unit well, and completing the start-up;
step six: when the vehicle is ready to stop, firstly, the regeneration function of the ionic liquid regeneration kettle is closed, then the feeding of ethanol and acetic acid of the reaction rectifying tower is cut off, the water-containing ionic liquid catalyst in the ionic liquid regeneration kettle is pumped into the acetic acid recovery tower through the control of a valve, the feeding of ethanol in the acetic acid recovery tower is stopped, and finally, the feeding of the ionic liquid in the reaction rectifying tower is cut off;
step seven: and finally, stopping the heating of the reboiler and the transportation of all pumps, well controlling the liquid levels of the reaction rectifying tower, the acetic acid recovery tower, the intermediate storage tank and the ionic liquid regeneration kettle, and waiting for the next start-up.
2. The original start-up and shutdown method for producing ethyl acetate by using the industrial ionic liquid catalyst as claimed in claim 1, characterized in that: the reaction rectifying tower is connected with the ionic liquid regeneration kettle through a pipeline, a pipeline flange is connected with a first valve, the reaction rectifying tower is connected with an acetic acid recovery tower through a pipeline, a second valve is connected with the pipeline flange, the acetic acid recovery tower is connected with the ionic liquid regeneration kettle through a pipeline, a fifth valve is connected with the pipeline flange, an ethanol feeding device is respectively connected with the reaction rectifying tower and the acetic acid recovery tower through a pipeline, the pipeline is respectively connected with a fourth valve and a third valve, the acetic acid recovery tower is connected with an intermediate storage tank through a pipeline, and the intermediate storage tank is connected with the ionic liquid regeneration kettle through a pipeline.
3. The original start-up and shutdown method for producing ethyl acetate by using the industrial ionic liquid catalyst as claimed in claim 1, characterized in that: in the second step, the fifth valve is opened, the first valve to the fourth valve are closed, and the ionic liquid content is analyzed by sampling at the bottom of the ionic liquid regeneration kettle at intervals, wherein the time depends on the regeneration capacity of the regeneration kettle and is fifteen to thirty minutes.
4. The original start-up and shutdown method for producing ethyl acetate by using the industrial ionic liquid catalyst as claimed in claim 1, characterized in that: in the third step, the boiling point of the ethyl acetate is seventy-seven ℃, and the ionic liquid content analyzed at the bottom of the ionic liquid regeneration kettle is higher than ninety-five percent, so that the product is qualified.
5. The original start-up and shutdown method for producing ethyl acetate by using the industrial ionic liquid catalyst as claimed in claim 1, characterized in that: in the fourth step, the time obtained by calculation according to the internal design of the reactive distillation column and the distance between the acetic acid feed port and the ionic liquid feed port is obtained after the specific time, the valves are switched, the first valve, the fourth valve and the fifth valve are opened, the second valve and the third valve are closed, and finally the time is obtained by calculation according to the internal design of the reactive distillation column and the distance between the ethanol feed port and the ionic liquid feed port.
6. The method for producing ethyl acetate by using the industrial ionic liquid catalyst to start and stop the vehicle originally according to claim 1, which is characterized in that: and a liquid level is arranged at the bottom of the reaction rectifying tower in the step five, the liquid level ranges from forty percent to seventy percent, the acetic acid recovery tower is controlled by a valve to start to feed ethanol, the bottom of the reaction rectifying tower starts to discharge materials to the acetic acid recovery tower, and the valves are in open states from the first valve to the fifth valve.
7. The method for producing ethyl acetate by using the industrial ionic liquid catalyst to start and stop the vehicle originally according to claim 1, which is characterized in that: in the sixth step, the feeding of the ethanol and the acetic acid in the reactive distillation column is cut off, namely the fourth valve is closed, the acetic acid feeding valve is closed, the second valve, the third valve and the fourth valve are closed through valve control, the first valve and the fifth valve are opened, and finally the feeding of the water-containing ionic liquid in the reactive distillation column and the acetic acid recovery column is cut off, namely the first valve and the fifth valve are closed.
8. The method for producing ethyl acetate by using the industrial ionic liquid catalyst to start and stop the vehicle originally according to claim 1, which is characterized in that: the ionic liquid is a mixture of seven components of pyridine, alkyl pyridine hydrogen sulfate and hydrogen phosphate, imidazole, alkyl imidazole hydrogen sulfate and hydrogen phosphate and free acid, and is a catalyst for catalyzing acidic substances and alcohol substances to react to produce ester substances.
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