CN212655719U - N-propyl acetate production system capable of recycling in grading manner - Google Patents
N-propyl acetate production system capable of recycling in grading manner Download PDFInfo
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- CN212655719U CN212655719U CN202020956686.2U CN202020956686U CN212655719U CN 212655719 U CN212655719 U CN 212655719U CN 202020956686 U CN202020956686 U CN 202020956686U CN 212655719 U CN212655719 U CN 212655719U
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- Prior art keywords
- ester
- phase separator
- raw material
- tank
- recovery
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- YKYONYBAUNKHLG-UHFFFAOYSA-N propyl acetate Chemical compound CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 238000004064 recycling Methods 0.000 title abstract description 4
- 150000002148 esters Chemical class 0.000 claims abstract description 70
- 239000002994 raw material Substances 0.000 claims abstract description 39
- 238000011084 recovery Methods 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002351 wastewater Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 230000005494 condensation Effects 0.000 claims abstract description 8
- 238000009833 condensation Methods 0.000 claims abstract description 8
- 229940090181 propyl acetate Drugs 0.000 claims abstract description 6
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000032050 esterification Effects 0.000 claims description 28
- 238000005886 esterification reaction Methods 0.000 claims description 28
- 238000004065 wastewater treatment Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 238000009776 industrial production Methods 0.000 abstract description 5
- 238000005191 phase separation Methods 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 13
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 10
- 239000000126 substance Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000009835 boiling Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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Abstract
The utility model relates to a hierarchical recovery returns propyl acetate production system who utilizes, the cauldron of esterifying is connected to a plurality of raw material tanks, the cauldron of esterifying connects gradually the condensation cooler, the dephasing ware, dephasing ware water meets the waste water dashpot, the waste water dashpot divides two way backward flow to connect to the cauldron of esterifying, receive the recovery tank, dephasing ware ester looks connects the crude ester dashpot, the crude ester dashpot divides two way to connect to the cauldron of esterifying, take off the light component and divide the tower bottom to connect the rectifying column lower part, the rectifying column top connects out to first ester cooler, first ester dephasing ware ester divides two way joint ester raw material tanks after meeting the rectifying dashpot, connect the rectifying column top, first ester dephasing ware water meets the recovery tank; the recovery tank is connected with a multi-stage flash evaporator through a pump. The concentrated head ester and the components are subjected to phase separation and repeated alcohol return for recycling, and are cooled and collected or partially returned for recycling after the concentration in the rectifying tower meets the requirements, so that the industrial production period can be ensured to meet the requirements of production efficiency and purity, the material return is also realized, and the production cost is favorably reduced.
Description
Technical Field
The utility model relates to a chemical production line, a hierarchical recovery returns propyl acetate production system who utilizes specifically says so.
Background
The present industrial production method mainly uses acetic acid and n-propanol as raw materials, and adopts the processes of esterification and rectification under the action of concentrated sulfuric acid catalyst to produce n-propyl acetate. And materials such as acetic acid, alcohol and the like brought out from the esterification kettle are refluxed to the esterification kettle from the bottom of the esterification kettle for continuous reaction. But the simple material returns for continuous reaction, wherein the content of the raw material substance is relatively low, and the raw material substance is directly returned for use, so that the industrial production period is increased, and the improvement of the production efficiency and the improvement of the purity are not facilitated.
Disclosure of Invention
The utility model provides a compact structure, the material returns usefulness, and reduction in production cost reduces wastewater discharge, can compromise a hierarchical recovery of industrial production efficiency and purity requirement and return propyl acetate production system who utilizes.
The utility model adopts the technical proposal that: the utility model provides a hierarchical recovery returns propyl acetate production system who utilizes, includes a plurality of raw material groove, esterification kettle, condensation cooler, phase separator, rectifying column, and esterification kettle is connected to a plurality of raw material groove, and esterification kettle connects gradually condensation cooler, phase separator, its characterized in that: the device comprises a phase separator, an esterification kettle, a recovery tank, a crude ester buffer tank, a light component removal tower, a rectification tower, a first ester cooler, a first ester phase separator, a second ester phase separator and a second ester phase separator, wherein the phase separator is connected with the wastewater buffer tank in a water-connection mode, the wastewater buffer tank is connected with the esterification kettle in a backflow mode in two ways, the other way is connected with the recovery tank, the phase separator is connected with the crude ester buffer tank in an ester-connection mode, the crude ester buffer tank is connected with the first ester phase separator in two ways in a backflow mode, the top of the first ester phase separator is connected with the rectification buffer tank in a ester-connection mode and then is connected with the second ester phase separator in; the bottom of the rectifying tower is connected with a discharge cooler which is connected with a finished product metering tank; the recovery tank is connected with a primary flash evaporator through a pump, the top of the primary flash evaporator is connected with a primary flash condenser, the primary flash condenser is connected with an ester raw material tank, the lower part of the primary flash evaporator is connected with a secondary flash evaporator through a pump, the top of the secondary flash evaporator is connected with a secondary flash condenser, the secondary flash condenser is connected back to the alcohol raw material tank, and the lower part of the secondary flash condenser is connected with a water discharge pipe; the head ester raw material groove and the alcohol return raw material groove are connected with the esterification kettle.
Further, the crude ester buffer tank is connected with a light component removal tower through a preheater.
Further, the drain pipe is connected with a wastewater treatment device.
Further, the drain pipe is connected back to the esterification kettle.
Acetic acid, normal propyl alcohol and sulfuric acid in a plurality of raw material tanks are metered and put into an esterification kettle, and are heated to generate normal propyl acetate and water, an azeotrope is formed in an esterification tower, the acetic acid, the normal propyl alcohol and the sulfuric acid are evaporated from the top of the tower, the acetic acid, the normal propyl alcohol and the sulfuric acid are cooled by a condensing cooler and then enter a phase separator for separation, a part of water phase flows back through a waste water buffer tank, a part of water phase flows back to a recovery tank to recover dissolved ester and alcohol, a part of ester phase flows back to the esterification tower through a crude ester buffer tank, a part of water phase enters a light component removal tower after being preheated by a preheater, the alcohol and the water are evaporated from the top of the light component removal tower, and the alcohol is recovered and; the tower bottom liquid of the light component removal tower is n-propyl acetate and some high boiling point substances, and is sent into a rectifying tower, alcohol, water and ester mixture head ester is separated from tower top components through rectification, after the head ester passes through a head ester cooler and a head ester phase separator, a part of the ester is sent into a rectifying buffer tank, and then a part of the ester is extracted and sent to a head ester raw material tank to be returned for esterification, and a part of the ester returns to the rectifying tower, when the bottom of the rectifying tower obtains finished products with qualified ester content, acidity and moisture, the discharged materials are sent into a finished product metering tank after being discharged and cooled. The recovery tank collects the wastewater containing ester and alcohol sent by the wastewater buffer tank and the head ester phase separator, the wastewater is pumped to the flash evaporator, the n-propyl acetate evaporated from the top of the evaporator is condensed by the flash condenser and then is connected to the alcohol raw material tank, and the wastewater is discharged from a drain pipe at the bottom of the tower.
The utility model discloses with the improvement of the structure that traditional cooling, split phase returned and utilize for concentrating first ester, component split phase return alcohol and return the utilization many times, concentration reaches the cooling collection or the partial utilization of returning after requiring in the rectifying column, when can ensure that the industrial production cycle satisfies production efficiency and purity requirement, compromise the material and return the usefulness, be favorable to reduction in production cost.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
In the figure: acetic acid raw material groove 1, n-propanol raw material groove 2, sulfuric acid raw material groove 3, head ester raw material groove 4, return alcohol raw material groove 5, esterification kettle 6, condensation cooler 7, phase separator 8, waste water buffer tank 9, crude ester buffer tank 10, preheater 11, lightness-removing component tower 12, lightness-removing condenser 13, rectifying tower 14, head ester cooler 15, head ester phase separator 16, rectifying buffer tank 17, discharge cooler 18, finished product metering tank 19, recovery tank 20, one-level flash evaporator 21, one-level flash condenser 22, second-level flash evaporator 23, second-level flash condenser 24, drain pipe 25.
Detailed Description
The following further description is made in conjunction with the accompanying drawings and examples.
FIG. 1 shows: the n-propyl acetate production system comprises an acetic acid raw material tank 1, an n-propanol raw material tank 2, a sulfuric acid raw material tank 3, a head ester raw material tank 4, an alcohol return raw material tank 5, an esterification kettle 6, a condensation cooler 7, a phase separator 8, a wastewater buffer tank 9, a crude ester buffer tank 10, a preheater 11, a light component removal tower 12, a light component removal condenser 13, a rectifying tower 14, a head ester cooler 15, a head ester phase separator 16, a rectifying buffer tank 17, a discharge cooler 18, a finished product metering tank 19, a recovery tank 20, a first-stage flash evaporator 21, a first-stage flash condenser 22, a second-stage flash evaporator 23, a second-stage flash condenser 24 and a drain pipe 25.
Acetic acid raw material tank 1, normal propyl alcohol raw material tank 2, sulfuric acid raw material tank 3, head ester raw material tank 4 and alcohol return raw material tank 5 are all connected with esterification reactor 6, esterification reactor 6 is connected with condensation cooler 7 and phase separator 8 in sequence, phase separator 8 is connected with waste water buffer tank 9 in water phase, waste water buffer tank 9 is divided into two paths and one path is returned to esterification reactor 6, another path is connected with recovery tank 20, phase separator 8 is connected with crude ester buffer tank 10 in ester phase, crude ester buffer tank 10 is divided into two paths and one path is returned to esterification reactor 6, another path is connected with lightness-removing component tower 12 through preheater 11, the top of lightness-removing component tower 12 is connected with lightness-removing condenser 13, lightness-removing condenser 13 is connected back to alcohol raw material tank 5, the bottom of lightness-removing component tower is connected with the lower part of rectifying tower 14, the top of rectifying tower 14 is connected to head ester cooler 15, head ester cooler 15 is connected with ester phase separator 16, the water phase of head ester phase separator is connected with recovery tank 20, ester phase is connected with rectifying tank 17, two paths are separated after rectifying buffer, connect ester raw material tank 4 all the way, another way backward flow connects to the rectifying column top, the ejection of compact of rectifying column bottom connects ejection of compact cooler 18, ejection of compact cooler connects finished product metering tank 19, recovery tank 20 connects one-level flash evaporator 21 through the pump, one-level flash evaporator top connects one-level flash condenser 22, one-level flash condenser connects ester raw material tank 4, one-level flash evaporator lower part pump connects second grade flash evaporator 23, second grade flash evaporator top connects second grade flash condenser 24, second grade flash condenser connects back mellow wine raw material tank 5, second grade flash condenser lower part connects drain pipe 25.
In the above embodiments, the chemical vessels such as the kettles, the tanks, the phase separators, and the towers are connected with a uniform channel pipeline, and the pipeline is provided with flow, valve control, and the like.
Claims (4)
1. The utility model provides a hierarchical recovery returns propyl acetate production system who utilizes, includes a plurality of raw material groove, esterification kettle, condensation cooler, phase separator, rectifying column, and esterification kettle is connected to a plurality of raw material groove, and esterification kettle connects gradually condensation cooler, phase separator, its characterized in that: the device comprises a phase separator, an esterification kettle, a recovery tank, a crude ester buffer tank, a light component removal tower, a rectification tower, a first ester cooler, a first ester phase separator, a second ester phase separator and a second ester phase separator, wherein the phase separator is connected with the wastewater buffer tank in a water-connection mode, the wastewater buffer tank is connected with the esterification kettle in a backflow mode in two ways, the other way is connected with the recovery tank, the phase separator is connected with the crude ester buffer tank in an ester-connection mode, the crude ester buffer tank is connected with the first ester phase separator in two ways in a backflow mode, the top of the first ester phase separator is connected with the rectification buffer tank in a ester-connection mode and then is connected with the second ester phase separator in; the bottom of the rectifying tower is connected with a discharge cooler which is connected with a finished product metering tank; the recovery tank is connected with a primary flash evaporator through a pump, the top of the primary flash evaporator is connected with a primary flash condenser, the primary flash condenser is connected with an ester raw material tank, the lower part of the primary flash evaporator is connected with a secondary flash evaporator through a pump, the top of the secondary flash evaporator is connected with a secondary flash condenser, the secondary flash condenser is connected back to the alcohol raw material tank, and the lower part of the secondary flash condenser is connected with a water discharge pipe; the head ester raw material groove and the alcohol return raw material groove are connected with the esterification kettle.
2. The n-propyl acetate production system for fractional recovery and recycle according to claim 1, wherein: the crude ester buffer tank is connected with a light component removal tower through a preheater.
3. The n-propyl acetate production system for fractional recovery and recycle according to claim 1, wherein: the drain pipe is connected with a wastewater treatment device.
4. The n-propyl acetate production system for fractional recovery and recycle according to claim 1, wherein: the water discharge pipe is connected back to the esterification kettle.
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CN202020956686.2U CN212655719U (en) | 2020-05-31 | 2020-05-31 | N-propyl acetate production system capable of recycling in grading manner |
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CN202020956686.2U CN212655719U (en) | 2020-05-31 | 2020-05-31 | N-propyl acetate production system capable of recycling in grading manner |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113717051A (en) * | 2021-09-16 | 2021-11-30 | 泰兴金江化学工业有限公司 | Preparation method of butyl acetate |
CN113880712A (en) * | 2021-09-16 | 2022-01-04 | 泰兴金江化学工业有限公司 | Preparation method of ethyl acetate |
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2020
- 2020-05-31 CN CN202020956686.2U patent/CN212655719U/en not_active Expired - Fee Related
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113717051A (en) * | 2021-09-16 | 2021-11-30 | 泰兴金江化学工业有限公司 | Preparation method of butyl acetate |
CN113880712A (en) * | 2021-09-16 | 2022-01-04 | 泰兴金江化学工业有限公司 | Preparation method of ethyl acetate |
CN113717051B (en) * | 2021-09-16 | 2023-08-04 | 泰兴金江化学工业有限公司 | Preparation method of butyl acetate |
CN113880712B (en) * | 2021-09-16 | 2023-08-04 | 泰兴金江化学工业有限公司 | Preparation method of ethyl acetate |
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CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20210305 |