CN216630349U - KA oil separator - Google Patents

KA oil separator Download PDF

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Publication number
CN216630349U
CN216630349U CN202123136879.7U CN202123136879U CN216630349U CN 216630349 U CN216630349 U CN 216630349U CN 202123136879 U CN202123136879 U CN 202123136879U CN 216630349 U CN216630349 U CN 216630349U
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membrane
tank
communicated
tower
collecting tank
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CN202123136879.7U
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徐徐
孙朋飞
高丽
王苏琴
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Jiangsu Liboxing Water Technology Co ltd
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Jiangsu Liboxing Water Technology Co ltd
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

Abstract

The application discloses a KA oil separation device which comprises a KA oil tank communicated with a membrane filtering device, wherein a clear liquid outlet of the membrane filtering device is communicated with an auxiliary heating tank after passing through refrigerant channels of a first heat exchanger and a second heat exchanger, the auxiliary heating tank is communicated with a membrane distillation device, a concentrated liquid outlet of the membrane distillation device is communicated with an extractive distillation tower, and a steam outlet of the extractive distillation tower is communicated with a cyclohexanone collecting tank through a heat medium channel of a first condenser; a discharge port at the bottom of the extraction and rectification tower is communicated with a hydroxyl-philic resin tank through a heating medium channel of a second condenser, two branch pipes are led out from the hydroxyl-philic resin tank and are respectively communicated with an extraction solvent tank and a cyclohexanol collecting tank, and the extraction solvent tank is communicated with the extraction and rectification tower; a steam outlet of the membrane distillation device is communicated with a cyclohexane collecting tank through a heating medium channel of the first heat exchanger; the cyclohexane collecting tank and the cyclohexanol collecting tank are both communicated with a vacuum device. The purposes of reducing energy consumption, water consumption and electric energy consumption can be achieved by utilizing the method.

Description

KA oil separator
Technical Field
The utility model relates to a KA oil separating device.
Background
KA oil is a product of cyclohexanone prepared by a cyclohexane oxidation method, and consists of a mixture of cyclohexane, cyclohexanol and cyclohexanone, and all components need to be separated in actual production. At present, a vacuum distillation method is mainly adopted for separating KA oil, a representative process is a three-tower combined separation process of a light component removal tower, a cyclohexanone rectification tower and a cyclohexanol rectification tower, the process is high in energy consumption and high in vacuum degree requirement, meanwhile, a large amount of electric energy, steam and circulating water are consumed, and the separation cost is high.
SUMMERY OF THE UTILITY MODEL
In order to solve the problems, the utility model provides a KA oil separator which comprises a KA oil tank, a membrane filtering device, an auxiliary heating tank, a membrane distillation device, an extractive distillation tower, a cyclohexanone collecting tank, a hydroxyl-philic resin tank, a cyclohexane collecting tank, a cyclohexanol collecting tank and a vacuum device, wherein a first discharge port of the KA oil tank is communicated with a second feed port of the membrane filtering device, a clear liquid outlet of the membrane filtering device is communicated with a third feed port of the auxiliary heating tank after sequentially passing through a refrigerant channel of a first heat exchanger and a refrigerant channel of a second heat exchanger, a third discharge port of the auxiliary heating tank is communicated with a fourth feed port of the membrane distillation device, a concentrated liquid outlet of the membrane distillation device is communicated with a fifth feed port of the extractive distillation tower through a conveying pump, and a vapor outlet at the top of the extractive distillation tower is communicated with a sixth feed port at the top of the cyclohexanone collecting tank through a heat medium channel of a first condenser;
a tower bottom discharge hole at the bottom of the extraction and rectification tower is connected with a tower bottom discharge pipe which is communicated with a seventh feed inlet at the top of the hydroxyl-philic resin tank through a heating medium channel of a second condenser, and a seventh discharge hole at the bottom of the hydroxyl-philic resin tank leads out two branch pipes which are respectively a cyclohexanol recovery branch pipe and an extraction solvent recovery branch pipe; an extraction solvent adding port at the upper part of the extraction rectifying tower is connected with an extraction solvent tank, and the extraction solvent recovery branch pipe is communicated with the extraction solvent tank; the cyclohexanol recovery branch pipe is communicated with an eighth feed inlet at the top of the cyclohexanol collecting tank through a heat medium channel of a third condenser; the top of the hydroxyl-philic resin tank is also provided with a hot air inlet pipe;
a steam outlet of the membrane distillation device is communicated with a ninth feed inlet at the top of the cyclohexane collecting tank after passing through a heating medium channel of the first heat exchanger; the upper part of the cyclohexane collecting tank is provided with a first vacuum interface, the upper part of the cyclohexanol collecting tank is provided with a second vacuum interface, and the first vacuum interface and the second vacuum interface are both connected to a vacuum suction port of a vacuum device.
In this application, adopt membrane distillation plant to replace traditional lightness-removing tower, replace traditional cyclohexanol rectifying column with the hydrophilic hydroxyl resin jar, reach the purpose that reduces the energy consumption, reduce water consumption and electric energy consumption. The vapor generated by the membrane distillation device is used for heating the KA oil raw material liquid through the first heat exchanger, so that the consumption of external energy is reduced, and meanwhile, the vapor is cooled and liquefied by utilizing the KA oil raw material liquid, so that the vapor is beneficial to recovery, two purposes are achieved, and the production cost is effectively reduced. Compared with the traditional process, the process has the advantages that the number of high-temperature rectifying towers is reduced, the vacuum degree requirement in the production process is reduced, and the production operation process is safer and simpler.
Furthermore, in order to improve the heat energy utilization rate and reduce the operation cost, a first condensate outlet of the first condenser, a second condensate outlet of the second condenser and a third condensate outlet of the third condenser are communicated with a heat medium channel of the second heat exchanger. And the waste heat obtained by the first condenser, the second condenser and the third condenser is used for heating the KA oil raw material liquid, so that the heat energy utilization efficiency is improved.
Furthermore, in order to accurately measure the amount of the extraction solvent entering the extraction and rectification tower, the extraction solvent tank is communicated with an extraction solvent adding port through a metering pump.
Furthermore, in order to ensure the rectification temperature in the extraction and rectification tower and the rectification effect, a reboiling pipe is led out from the tower bottom discharge pipe, the reboiling pipe is connected with a tower kettle reboiler, and a reboiling liquid outlet on the tower kettle reboiler is communicated with a reboiling liquid inlet at the bottom of the extraction and rectification tower.
Furthermore, in order to reduce energy waste and avoid local overheating, a heating jacket is arranged on the outer wall of the auxiliary heating tank, and a stirrer is arranged in the auxiliary heating tank.
Specifically, in order to ensure the filtering effect, the filtering membrane in the membrane filtering device is an ultrafiltration membrane or a microfiltration membrane, the filtering membrane is in a flat plate membrane or a tubular membrane, and the material of the filtering membrane is a ceramic membrane or a polytetrafluoroethylene membrane.
Specifically, in order to ensure the distillation effect, the membrane distillation device adopts a vacuum type membrane distillation device, a filtering membrane in the membrane distillation device is an ultrafiltration membrane or a nanofiltration membrane, the filtering membrane is in a flat plate membrane or a tubular membrane, and the filtering membrane is made of a ceramic membrane or a polytetrafluoroethylene membrane.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment of the present invention.
Detailed Description
Referring to fig. 1, a KA oil separator includes a KA oil tank 1, a membrane filtering device 2, an auxiliary heating tank 3, a membrane distillation device 4, an extractive distillation tower 5, a cyclohexanone collection tank 6, a hydroxyl-philic resin tank 7, a cyclohexanol collection tank 8, a cyclohexane collection tank 9, and a vacuum device 18, wherein a first discharge port 12 of the KA oil tank 1 is communicated with a second feed port 21 of the membrane filtering device 2, and a purified liquid outlet 22 of the membrane filtering device 2 is communicated with a third feed port 31 on the upper portion of the auxiliary heating tank 3 after sequentially passing through a refrigerant channel of a first heat exchanger 201 and a refrigerant channel of a second heat exchanger 202. A heating jacket 35 is arranged on the outer wall of the auxiliary heating tank 3, a stirrer 33 is arranged in the auxiliary heating tank, the stirring of the stirrer extends upwards out of the top of the auxiliary heating tank 3, and then a driving motor 34 is arranged and fixedly arranged on the top of the auxiliary heating tank 3.
The third discharge port 32 at the bottom of the auxiliary heating tank 3 is communicated with the fourth feed port 41 of the membrane distillation device 4, the concentrated solution outlet 43 of the membrane distillation device 4 is communicated with the fifth feed port 51 of the extractive distillation tower 5 through a delivery pump 507, and the vapor outlet 53 at the top of the extractive distillation tower is communicated with the sixth feed port 61 at the top of the cyclohexanone collecting tank 6 through a heat medium channel of the first condenser 531. The first condensate outlet 532 of the first condenser 531 is communicated with the heating medium inlet 203 of the second heat exchanger 202.
A first feed port 11 is provided in the top of the KA oil tank 1, and a raw material pipe 10 is connected to the first feed port 11. A cyclohexanone discharge valve 63 is arranged at a sixth discharge port 62 at the bottom of the cyclohexanone collecting tank 6.
The tower bottom discharge port 54 at the bottom of the extractive distillation tower 5 is connected with a tower bottom discharge pipe 57, the tower bottom discharge pipe 57 is communicated with the seventh feed port 71 at the top of the hydroxyl-philic resin tank 7 through a heat medium channel of the second condenser 56, a third switching valve 562 is arranged on the tower bottom discharge pipe 57, and a second condensate outlet 561 of the second condenser 56 is communicated with the heat medium inlet 203 of the second heat exchanger 202. A reboiling pipe 542 is led out from the material outlet pipe at the bottom of the tower, a tower kettle reboiler 541 is connected to the reboiling pipe, and a reboiling liquid outlet 543 at the upper end of the tower kettle reboiler 541 is communicated with a reboiling liquid inlet 55 at the bottom of the extraction rectifying tower 5. The connection point of the reboiling pipe and the column bottom outlet pipe is located between the column bottom outlet 54 and the third switching valve 562.
A seventh discharge port 73 at the bottom of the hydrophilic resin tank 7 leads out two branch pipes which are a cyclohexanol recovery branch pipe 731 and an extraction solvent recovery branch pipe 732, respectively. A hot air inlet 72 is provided at the top of the hydrophilic resin tank 7, and a hot air inlet pipe 74 is connected to the hot air inlet 72 for introducing hot air into the hydrophilic resin tank 7.
The extraction solvent recovery branch pipe 732 is connected to the solvent recovery port 502 at the top of the extraction solvent tank 501, and a second switching valve 734 is attached to the extraction solvent recovery branch pipe 732. The solvent outlet 503 at the bottom of the extraction solvent tank 501 is communicated with the extraction solvent adding port 52 at the upper part of the extractive distillation column through a metering pump 505. An extraction solvent replenishment pipe 504 is connected to the top of the extraction solvent tank 501 for replenishing the extraction solvent tank with fresh extraction solvent.
The cyclohexanol recovery branch pipe 731 is connected to the eighth feed port 81 at the top of the cyclohexanol collection tank 8 via a heat medium passage of the third condenser 16, and a first switching valve 733 is installed in the cyclohexanol recovery branch pipe 731. The third condensate outlet 163 of the third condenser 16 is communicated with the heating medium inlet 203 of the second heat exchanger 202. A discharge valve 84 is installed at an eighth discharge port 82 at the bottom of the cyclohexanol collecting tank 8.
The vapor outlet 42 of the membrane distillation device 4 is communicated with the ninth feed inlet 91 at the top of the cyclohexane collecting tank 9 after passing through the heat medium channel of the first heat exchanger 201. A discharge valve 94 is arranged at a ninth discharge hole 93 at the bottom of the cyclohexane collecting tank 9.
The upper part of the side wall of the cyclohexane collecting tank 9 is provided with a first vacuum interface 92, the upper part of the side wall of the cyclohexanol collecting tank 8 is provided with a second vacuum interface 83, and the first vacuum interface and the second vacuum interface are both connected to a vacuum suction port 180 of the vacuum device 18. In the present embodiment, the first vacuum port 92 is connected to the vacuum suction port 180 via a first vacuum tube 181, and a first regulating valve 183 is mounted on the first vacuum tube 181. The second vacuum port 83 is connected to the vacuum port 180 via a second vacuum tube 182, and a second regulator valve 184 is mounted on the second vacuum tube 182.
Specifically, in this embodiment, the filtering membrane in the membrane filtering device is a flat membrane, and the flat membrane is an ultrafiltration membrane made of ceramic, that is, the flat membrane is a ceramic ultrafiltration membrane. It is understood that in other embodiments, the form of the filtering membrane in the membrane filtering device can also adopt a tubular membrane, that is, the form of the filtering membrane can be a flat plate membrane or a tubular membrane; the material of the filtering membrane can also be a polytetrafluoroethylene membrane; and a microfiltration membrane can be adopted as the filtering membrane according to the particle size of the impurities in the KA oil.
In this embodiment, the membrane distillation apparatus is a vacuum membrane distillation apparatus, and the filtering membrane in the membrane distillation apparatus is a flat membrane, which is an ultrafiltration membrane made of ceramic material, that is, the flat membrane is a ceramic ultrafiltration membrane. It is understood that in other embodiments, the form of the filtering membrane in the membrane distillation device can also adopt a tubular membrane, that is, the form of the filtering membrane can be a flat membrane or a tubular membrane; the material of the filtering membrane can also be a polytetrafluoroethylene membrane; according to the distillation requirement, the filter membrane can also adopt a nanofiltration membrane according to the aperture.
When the working of the embodiment, the KA oil raw material liquid enters the KA oil tank 1 through the raw material pipe 10, and the KA oil raw material liquid in the KA oil tank 1 sequentially enters the auxiliary heating tank 3 through the membrane filtering device 2, the first heat exchanger 201 and the second heat exchanger 202; when the KA oil separation device is just started, the KA oil raw material liquid is completely heated by the auxiliary heating tank, after the KA oil separation device operates normally, the KA oil raw material liquid can be heated by the first heat exchanger 201 and the second heat exchanger 202, and the auxiliary heating tank 3 only plays a role in supplementary heating.
The KA oil feedstock discharged from the auxiliary heating tank 3 enters the membrane distillation apparatus 4 for distillation and concentration, and the vapor discharged from the vapor outlet 42 of the membrane distillation apparatus 4 serves as a heat source for the first heat exchanger. The heat source of the second heat exchanger is the condensed water discharged from the first condenser 531, the first condenser 56, and the third condenser 16.
The vapor discharged from the permeation side of the membrane distillation device 4 is cyclohexane vapor, the cyclohexane collection tank 9 is in a negative pressure state under the action of the vacuum device 18, and under the action of the negative pressure, the cyclohexane vapor exchanges heat with the KA oil raw material liquid through the first heat exchanger 201, is condensed and liquefied, then enters the cyclohexane collection tank 9 to be collected, and is periodically discharged through the ninth discharge hole 93.
Liquid discharged from a concentrated solution outlet 43 of the membrane distillation device 4 enters the extractive distillation tower 5 through a delivery pump 507, and the extraction solvent in the extraction solvent tank 501 enters the extractive distillation tower 5 through a metering pump 505 for extractive distillation; the cyclohexanone vapor discharged from the top of the extractive distillation column 5 is cooled and liquefied by the first condenser 531, and automatically flows into the cyclohexanone collection tank 6 under the action of gravity.
The tower bottom liquid at the bottom of the extractive distillation tower 5 firstly enters the reboiler 541, is heated by the reboiler, and then flows back to the extractive distillation tower from the reboiler outlet 543 through the reboiled liquid inlet 55, and is circulated continuously until the specified time is reached, and the third switching valve 562 is in a closed state during the operation; after the circulating reboiling reaches the set time, the reboiler 541 stops working, at this time, the third switching valve 562 is opened, and the tower bottom liquid after the extractive distillation enters the hydroxyl-philic resin tank 7 through the heat medium channel of the second condenser 56; after the bottom liquid is added, the third switching valve 562 is closed, the reboiler is restarted, and the circulation and reboiling are continued, and the process is circulated according to the above steps. In a hydrophilic hydroxyl resin tank 7, the tower bottom liquid is adsorbed on the hydrophilic hydroxyl resin under the hydrogen bonding action of the hydrophilic hydroxyl resin; the bottom liquid from which cyclohexanol is removed becomes post-adsorption liquid, the main components of the post-adsorption liquid are extraction solvent, a small amount of cyclohexanol and a small amount of residual cyclohexanone, the post-adsorption liquid is returned to the extraction solvent tank 501 through an extraction solvent recovery branch pipe 732 for recycling, and the consumed extraction solvent is periodically replenished into the extraction solvent tank 501 through an extraction solvent replenishment pipe 504.
After the adsorption of the hydrophilic hydroxyl resin in the hydrophilic hydroxyl resin tank 7 is completed, emptying the solution in the tank, introducing hot air into the hydrophilic hydroxyl resin tank 7 through a hot air inlet pipe 74, heating the hydrophilic hydroxyl resin, destroying the hydrogen bond between cyclohexanol and the hydrophilic hydroxyl resin under the negative pressure condition, and removing the cyclohexanol adsorbed on the hydrophilic hydroxyl resin, wherein the temperature of the hot air is 90-105 ℃. At this time, the second switching valve 734 is in a closed state, and the first switching valve 733 is in an open state. Under the action of the vacuum device 18, the interior of the cyclohexanol collecting tank 8 is in a negative pressure state, and under the action of the negative pressure, cyclohexanol desorbed from the hydrophilic resin enters the cyclohexanol collecting tank 8 after being condensed by the third condenser 16.

Claims (7)

1. A KA oil separation device is characterized by comprising a KA oil tank, a membrane filtering device, an auxiliary heating tank, a membrane distillation device, an extractive distillation tower, a cyclohexanone collecting tank, a hydroxyl-philic resin tank, a cyclohexane collecting tank, a cyclohexanol collecting tank and a vacuum device, wherein a first discharge port of the KA oil tank is communicated with a second feed port of the membrane filtering device, a clear liquid outlet of the membrane filtering device is communicated with a third feed port of the auxiliary heating tank after sequentially passing through a refrigerant channel of a first heat exchanger and a refrigerant channel of a second heat exchanger, a third discharge port of the auxiliary heating tank is communicated with a fourth feed port of the membrane distillation device, a concentrated liquid outlet of the membrane distillation device is communicated with a fifth feed port of the extractive distillation tower through a conveying pump, and a vapor outlet at the top of the extractive distillation tower is communicated with a sixth feed port at the top of the cyclohexanone collecting tank through a heat medium channel of a first condenser;
a tower bottom discharge hole at the bottom of the extraction and rectification tower is connected with a tower bottom discharge pipe which is communicated with a seventh feed inlet at the top of the hydroxyl-philic resin tank through a heating medium channel of a second condenser, and a seventh discharge hole at the bottom of the hydroxyl-philic resin tank leads out two branch pipes which are respectively a cyclohexanol recovery branch pipe and an extraction solvent recovery branch pipe; an extraction solvent adding port at the upper part of the extraction rectifying tower is connected with an extraction solvent tank, and the extraction solvent recovery branch pipe is communicated with the extraction solvent tank; the cyclohexanol recovery branch pipe is communicated with an eighth feed inlet at the top of the cyclohexanol collecting tank through a heat medium channel of a third condenser; the top of the hydroxyl-philic resin tank is also provided with a hot air inlet pipe;
a steam outlet of the membrane distillation device is communicated with a ninth feed inlet at the top of the cyclohexane collecting tank after passing through a heating medium channel of the first heat exchanger; the upper part of the cyclohexane collecting tank is provided with a first vacuum interface, the upper part of the cyclohexanol collecting tank is provided with a second vacuum interface, and the first vacuum interface and the second vacuum interface are both connected to a vacuum suction port of a vacuum device.
2. The KA oil separator of claim 1, wherein the first condensate outlet of the first condenser, the second condensate outlet of the second condenser, and the third condensate outlet of the third condenser are all in communication with the heat medium passage of the second heat exchanger.
3. The KA oil separating device of claim 1, wherein the extraction solvent tank communicates with the extraction solvent addition port via a metering pump.
4. The KA oil separator of claim 1, wherein a reboiler is provided in the bottoms outlet pipe, and a reboiler is connected to the reboiler, and the reboiler outlet of the reboiler is connected to the reboiler inlet of the bottom of the extractive distillation column.
5. The KA oil separation device according to claim 1, wherein a heating jacket is provided on an outer wall of the auxiliary heating tank, and an agitator is installed in the auxiliary heating tank.
6. The KA oil separator of claim 1, wherein the filtration membrane in the membrane filtration device is an ultrafiltration membrane or a microfiltration membrane, the filtration membrane is in the form of a flat membrane or a tubular membrane, and the filtration membrane is made of a ceramic membrane or a polytetrafluoroethylene membrane.
7. The KA oil separator according to claim 1, wherein the membrane distillation device is a vacuum type membrane distillation device, the filtering membrane in the membrane distillation device is an ultrafiltration membrane or a nanofiltration membrane, the filtering membrane is in the form of a flat plate membrane or a tubular membrane, and the filtering membrane is made of a ceramic membrane or a polytetrafluoroethylene membrane.
CN202123136879.7U 2021-12-14 2021-12-14 KA oil separator Active CN216630349U (en)

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Application Number Priority Date Filing Date Title
CN202123136879.7U CN216630349U (en) 2021-12-14 2021-12-14 KA oil separator

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Application Number Priority Date Filing Date Title
CN202123136879.7U CN216630349U (en) 2021-12-14 2021-12-14 KA oil separator

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CN216630349U true CN216630349U (en) 2022-05-31

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