CN220245678U - Solid-liquid separation system of iodine-containing acetic acid waste liquid - Google Patents

Solid-liquid separation system of iodine-containing acetic acid waste liquid Download PDF

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Publication number
CN220245678U
CN220245678U CN202321003629.2U CN202321003629U CN220245678U CN 220245678 U CN220245678 U CN 220245678U CN 202321003629 U CN202321003629 U CN 202321003629U CN 220245678 U CN220245678 U CN 220245678U
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valve
liquid
concentrated solution
membrane tube
waste liquid
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CN202321003629.2U
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王忠华
段红宇
赵禄强
黄力
金贻星
李源
徐顺
王素芹
万立阳
赵铁均
顾雄毅
田义斌
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Jiangsu Jicui Topso Clean Energy R & D Co ltd
JIANGSU SOPO (GROUP) CO Ltd
JIANGSU SOPO CHEMICAL CO LTD
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Jiangsu Jicui Topso Clean Energy R & D Co ltd
JIANGSU SOPO (GROUP) CO Ltd
JIANGSU SOPO CHEMICAL CO LTD
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Abstract

The utility model provides a solid-liquid separation system of iodine-containing acetic acid waste liquid, which comprises a membrane tube filter, a concentrated solution storage tank and a centrifuge, wherein the acetic acid waste liquid containing iodine simple substances is injected into the membrane tube filter and filtered by the membrane tube filter to form concentrated solution, and the concentrated solution is stored in the concentrated solution storage tank; after a certain amount of concentrated solution is collected in the concentrated solution storage tank, the concentrated solution is injected into a centrifugal machine; after centrifugal separation by a centrifugal machine, separating into iodine simple substance and centrifugal clear liquid, loading the iodine simple substance into a collecting bag through a fifth valve, and injecting the centrifugal clear liquid into a membrane tube filter through a liquid return tube. The desalted water in the back flush water tank enters the membrane tube filter to back flush the membrane tube filter. According to the utility model, the content of iodine simple substance in the filtered concentrated solution is controlled by controlling the flow of the inlet and the outlet of the membrane tube filter, so that the high-efficiency separation, energy conservation and consumption reduction of a subsequent centrifugal machine are ensured.

Description

Solid-liquid separation system of iodine-containing acetic acid waste liquid
Technical Field
The utility model relates to the technical field of solid-liquid separation, in particular to a solid-liquid separation system for iodine-containing acetic acid waste liquid.
Background
The industrial production method of acetic acid mainly uses a methanol carbonylation method, the process uses methanol and CO as raw materials, rhodium chloride as a catalyst and methyl iodide as a cocatalyst, crude acetic acid is synthesized under the conditions of 2.5-3 MPa and 180-190 ℃, and then the crude acetic acid is purified by a rectification procedure to obtain the finished product acetic acid. During the production process, a certain amount of acetic acid waste liquid containing I-is generated. Currently, the industry mainly adopts an incineration method to treat acetic acid waste liquid. However, iodine cannot be converted in the incineration process, purple smoke is formed, and direct incineration causes great environmental pollution. And, more, a waste of resources.
The utility model patent application with the application publication number of CN113636687A discloses a recycling process of high-value chemicals in acetic acid plant wastewater. The process converts iodide in the acetic acid production wastewater into iodine simple substance through an iodide conversion unit, and then the iodine simple substance is separated from the acetic acid production wastewater through a solid-liquid separation system, so that the process is a novel recycling technology of I-in the acetic acid waste liquid. In order to realize the industrialization of the technology, a scientific and reasonable solid-liquid separation system of iodine simple substance in the acetic acid waste liquid needs to be designed. The solid-liquid separation system disclosed in this application adopts a membrane tube filtration enrichment device and a centrifugal dehydration treatment process, but no specific scheme of the solid-liquid separation system is given, and therefore, it is necessary to provide a solid-liquid separation system capable of realizing separation of acetic acid waste liquid containing iodine simple substance.
Disclosure of Invention
The technical problems to be solved by the utility model are as follows: in order to overcome the defects in the prior art, the utility model provides the solid-liquid separation system for the acetic acid waste liquid containing iodine, which can realize the efficient separation of the iodine simple substance in the acetic acid waste liquid and has the characteristics of simple design and simple operation.
The technical scheme adopted for solving the technical problems is as follows: the solid-liquid separation system comprises a membrane tube filter, a concentrated solution storage tank and a centrifuge, wherein a waste liquid inlet, a clear liquid outlet and a concentrated solution outlet are formed in the membrane tube filter, a waste liquid inlet pipe for introducing the iodine-containing acetic acid waste liquid is arranged on the waste liquid inlet, a first valve is arranged on the waste liquid inlet pipe and used for controlling the on-off of the waste liquid inlet pipe, a clear liquid outlet pipe for leading out acetic acid solution after iodine filtration is arranged on the clear liquid outlet, a concentrated solution first outlet pipe is arranged on the concentrated solution outlet, the other end of the concentrated solution first outlet pipe is connected to a liquid inlet of the concentrated solution storage tank, a liquid outlet of the concentrated solution storage tank is connected to a liquid inlet of the centrifuge through a concentrated solution second outlet pipe, and a fourth valve is arranged on the concentrated solution second outlet pipe and used for controlling the on-off of the concentrated solution second outlet pipe; the centrifugal machine is also provided with a solid outlet and a liquid return port for discharging solid iodine, the solid outlet is used for discharging solid iodine simple substances separated by the centrifugal machine, the solid outlet is also provided with a solid outlet pipe, the solid outlet pipe is provided with a fifth valve for controlling the on-off of the solid outlet pipe, and the solid iodine simple substances enter the collecting bag through the fifth valve on the solid outlet pipe; the liquid return port is provided with a liquid return pipe, the other end of the liquid return pipe is connected to the waste liquid inlet pipe, the liquid return pipe is provided with a third valve, and the third valve is used for controlling the on-off of the liquid return pipe.
If the acetic acid waste liquid filtered by the membrane tube filter directly enters the centrifuge, on one hand, the centrifuge is always in a working state, so that the problem of higher energy consumption exists, and on the other hand, the content of iodine in the filtrate is lower, and the separation efficiency is lower.
Further, in order to realize flow control on the inlet and the outlet of the membrane tube filter, the membrane tube filter further comprises a sixth valve and a seventh valve, wherein the sixth valve is arranged on the clear liquid outlet pipe, the seventh valve is arranged on the waste liquid inlet pipe between the first valve and the waste liquid inlet, the sixth valve is used for controlling the flow of the clear liquid outlet, and the seventh valve is used for controlling the flow of the waste liquid inlet. The outlet flow and the inlet flow of the membrane tube filter are controlled through a sixth valve and a seventh valve, so that the concentration of iodine simple substance in the filtered acetic acid waste liquid is improved, and the filtering efficiency of the centrifugal machine is improved; meanwhile, when the concentration of the iodine simple substance in the acetic acid waste liquid does not reach the preset concentration, no acetic acid waste liquid directly enters the centrifugal machine, and at the moment, the centrifugal machine is in an unoperated state, so that the energy consumption can be saved. The filtered concentrated solution is firstly stored in a concentrated solution storage tank, and enters a centrifugal machine for separation after a certain amount of concentrated solution is reached,
preferably, the ratio of the flow rate of the clear liquid outlet to the flow rate of the waste liquid inlet is controlled to be 0.7-0.9. As a further preferable mode, the ratio of the flow rate of the clear liquid outlet to the flow rate of the waste liquid inlet is controlled to be 0.8-0.9. The flow of the clear liquid outlet is smaller than that of the waste liquid inlet, so that a certain pressure difference exists between the inlet and the outlet, and the membrane tube filter has better filtering effect; in addition, the content of iodine simple substance in the formed concentrated solution can be effectively controlled through the ratio of the flow, so that the concentration of the concentrated solution is adjusted, and the separation efficiency of a subsequent centrifugal machine is improved.
Further, in order to ensure the filtering effect of the membrane tube filter, the membrane tube filter further comprises a differential pressure meter and a back flushing water tank, wherein the differential pressure meter is connected in parallel with the two ends of an inlet and an outlet of the membrane tube filter and used for detecting the differential pressure of the front end and the back end of the membrane tube filter, the membrane tube filter is further provided with a back flushing liquid inlet, the back flushing water tank is connected to the back flushing liquid inlet of the membrane tube filter through a back flushing pipe, and a second valve is arranged on a pipeline between the back flushing water tank and the back flushing liquid inlet. When back flushing is carried out, the second valve is opened, and after the back flushing is finished, the second valve is closed, so that the membrane tube filter can be normally used for solid-liquid separation.
Further, the membrane tube in the membrane tube filter is made of ceramics, siC or Al 2 O 3 . Acetic acid waste liquid enters a tube side of the membrane tube filter; preferably, the pore diameter of the membrane tube in the membrane tube filter is 3. Mu.m.
Further, the solid-liquid separation system of the iodine-containing acetic acid waste liquid further comprises a control unit, and the control unit is connected with each component in the solid-liquid separation system through a circuit so as to realize automatic control. The control unit is connected with the centrifugal machine, the differential pressure gauge and each valve through lines to transmit and control signals so as to realize automatic control of the centrifugal machine, the differential pressure gauge and each valve.
The solid-liquid separation method of the iodine-containing acetic acid waste liquid adopts the solid-liquid separation system of the iodine-containing acetic acid waste liquid, and further comprises the following steps:
s1: opening a first valve and a seventh valve, and injecting acetic acid waste liquid containing iodine simple substance into the membrane tube filter;
s2: the sixth valve is opened, so that the clear liquid filtered by the membrane tube filter is discharged from the clear liquid outlet tube and can directly enter the subsequent treatment process of the acetic acid waste liquid;
s3: filtering the acetic acid waste liquid by a membrane tube filter to form concentrated solution, and when the iodine simple substance in the concentrated solution is at least 10 times of the initial concentration, allowing the concentrated solution to enter a concentrated solution storage tank; further preferably, the concentration of the elemental iodine in the waste liquid entering the concentrated solution storage tank is 10 to 20 times the initial concentration.
S4: after the amount of the concentrated solution collected in the concentrated solution storage tank meets the separation amount of the centrifuge, opening a fourth valve, injecting the concentrated solution into the centrifuge, closing the fourth valve after the concentrated solution is completely injected into the centrifuge, and then starting the centrifuge; the range of the separation amount of the centrifugal machine is related to parameters of the centrifugal machine, so that the amount of concentrated liquid reaches the maximum amount which can be separated each time of the centrifugal machine as much as possible, the working efficiency of the centrifugal machine can be ensured, frequent starting is not needed, and the purposes of energy conservation and consumption reduction are achieved.
S5: separating iodine simple substance from the concentrated solution after centrifugation by a centrifugal machine, and forming centrifugal clear liquid; after separation is completed, the centrifugal machine is stopped, a fifth valve on a solid outlet pipe is opened, and iodine simple substances are filled into a collecting bag; simultaneously, the third valve is opened, and the centrifugal clear liquid is injected into the membrane tube filter through the liquid return tube. After separation by the centrifuge, the centrifugal clear liquid cannot be ensured to completely contain no iodine simple substance, so that the centrifugal clear liquid is re-injected into the membrane tube filter for circulating filtration in order to ensure the filtering and separating effects. The opening of the third valve and the fifth valve is not sequentially limited.
In the process, the membrane tube filter is always in a working state.
Further, the method further comprises the step of back flushing, wherein when the membrane tube filter is used for filtering, the differential pressure gauge is used for detecting the differential pressure of the front end and the rear end of the membrane tube filter, when the differential pressure of the front end and the rear end of the membrane tube filter reaches 50-150 kPa, back flushing operation is carried out, at the moment, the fourth valve, the sixth valve and the seventh valve are closed, the second valve is opened, flushing fluid in a back flushing water tank enters the membrane tube filter through a back flushing pipe, back flushing is carried out on the membrane tube filter, after flushing is carried out for 10min, the second valve is closed, the fourth valve, the sixth valve and the seventh valve are opened, and solid-liquid separation operation is continued.
Further, the time of each back flushing operation is 5-10 min.
Further, the flow rate of desalted water for each backwashing is 3-5 times of the feed flow rate of the membrane tube filter.
The beneficial effects of the utility model are as follows:
(1) According to the solid-liquid separation system of the acetic acid waste liquid containing the iodine simple substance, disclosed by the utility model, a solid-liquid separation mode of combining the membrane tube filter with the centrifugal machine is adopted, the membrane tube filter is used for concentrating the iodine simple substance in the acetic acid waste liquid, the centrifugal machine is used for separating the iodine simple substance from the concentrated solution, and the iodine simple substance in the acetic acid waste liquid can be completely separated through the system, so that the influence of the iodine simple substance on a downstream process of disposal of the acetic acid waste liquid is avoided.
(2) According to the solid-liquid separation system for the acetic acid waste liquid containing iodine simple substance, disclosed by the utility model, the flow of the inlet valve and the outlet valve of the membrane tube filter is controlled to be in a certain ratio through the automatic control system, so that the concentration effect of the membrane tube filter is ensured.
Drawings
The utility model is further described below with reference to the drawings and examples.
Fig. 1 is a schematic structural view of a preferred embodiment of the present utility model.
In the figure: 1-membrane tube filter, 2-back flush water pitcher, 3-concentrate storage tank, 4-centrifuge, 5-first valve, 6-second valve, 7-third valve, 8-fourth valve, 9-fifth valve, 10-sixth valve, 11-seventh valve, 12-waste liquid inlet pipe, 13-clear liquid outlet pipe, 14-concentrate first outlet pipe, 15-concentrate second outlet pipe, 16-return pipe, 17-back flush pipe.
Detailed Description
The utility model will now be described in further detail with reference to the accompanying drawings. The drawings are simplified schematic representations which merely illustrate the basic structure of the utility model and therefore show only those features which are relevant to the utility model, and orientation and reference (e.g., up, down, left, right, etc.) may be used solely to aid in the description of the features in the drawings. The following detailed description is, therefore, not to be taken in a limiting sense, and the scope of the claimed subject matter is defined only by the appended claims and equivalents thereof.
As shown in fig. 1, the solid-liquid separation system of the iodine-containing acetic acid waste liquid comprises a membrane tube filter 1, a concentrated solution storage tank 3 and a centrifuge 4, wherein the membrane tube filter 1 is provided with a waste liquid inlet, a clear solution outlet and a concentrated solution outlet, the waste liquid inlet is provided with a waste liquid inlet tube 12 for introducing the iodine-containing acetic acid waste liquid, the waste liquid inlet tube 12 is provided with a first valve 5, the first valve 5 is used for controlling the on-off of the waste liquid inlet tube 12, the clear solution outlet is provided with a clear solution outlet tube 13 for leading out an acetic acid solution after iodine filtration, the concentrated solution outlet is provided with a concentrated solution first outlet tube 14, the other end of the concentrated solution first outlet tube 14 is connected to a liquid inlet of the concentrated solution storage tank 3, a liquid outlet of the concentrated solution storage tank 3 is connected to a liquid inlet of the centrifuge 4 through a concentrated solution second outlet tube 15, the concentrated solution second outlet tube 15 is provided with a fourth valve 8, and the fourth valve 8 is used for controlling the on-off of the concentrated solution second outlet tube 15; the centrifugal machine 4 is also provided with a solid outlet and a liquid return port for discharging solid iodine, the solid outlet is used for discharging solid iodine simple substances separated by the centrifugal machine 4, the solid outlet is also provided with a solid outlet pipe, the solid outlet pipe is provided with a fifth valve 9 for controlling the on-off of the solid outlet pipe, and the solid iodine simple substances enter the collecting bag through the fifth valve 9 on the solid outlet pipe; the liquid return port is provided with a liquid return pipe 16, the other end of the liquid return pipe 16 is connected to the waste liquid inlet pipe 12, the liquid return pipe 16 is provided with a third valve 7, and the third valve 7 is used for controlling the on-off of the liquid return pipe 16.
In order to realize the flow control on the inlet and the outlet of the membrane tube filter 1, the membrane tube filter further comprises a sixth valve 10 and a seventh valve 11, wherein the sixth valve 10 is arranged on a clear liquid outlet pipe 13, the seventh valve 11 is arranged on a waste liquid inlet pipe 12 between the first valve 5 and the waste liquid inlet, the sixth valve 10 is used for controlling the clear liquid outlet flow, and the seventh valve 11 is used for controlling the waste liquid inlet flow. Preferably, the ratio of the flow rate of the clear liquid outlet to the flow rate of the waste liquid inlet is controlled to be 0.7-0.9. As a further preferable mode, the ratio of the flow rate of the clear liquid outlet to the flow rate of the waste liquid inlet is controlled to be 0.8-0.9.
In order to ensure the filtering effect of the membrane tube filter 1, the membrane tube filter further comprises a differential pressure meter and a back flushing water tank 2, wherein the differential pressure meter is connected in parallel with the two ends of an inlet and an outlet of the membrane tube filter 1 and is used for detecting the differential pressure of the front end and the back end of the membrane tube filter 1, the membrane tube filter 1 is further provided with a back flushing liquid inlet, the back flushing water tank 2 is connected to the back flushing liquid inlet of the membrane tube filter 1 through a back flushing pipe 17, and a second valve 6 is arranged on a pipeline between the back flushing water tank 2 and the back flushing liquid inlet. When back flushing is carried out, the second valve 6 is opened, and after the back flushing is finished, the second valve 6 is closed, so that the membrane tube filter 1 can be normally used for solid-liquid separation. The membrane tube in the membrane tube filter 1 is made of ceramics, siC or Al 2 O 3 . Acetic acid waste liquid enters a tube side of the membrane tube filter 1; preferably, the pore diameter of the membrane tube in the membrane tube filter 1 is 3. Mu.m.
The solid-liquid separation system of the iodine-containing acetic acid waste liquid further comprises a control unit, wherein the control unit is connected with each component in the solid-liquid separation system through a circuit so as to realize automatic control. The control unit centrifuge 4, the differential pressure gauge and each valve are connected through a circuit to transmit and control signals so as to realize automatic control of the centrifuge 4, the differential pressure gauge and each valve.
The solid-liquid separation method of the iodine-containing acetic acid waste liquid adopts the solid-liquid separation system of the iodine-containing acetic acid waste liquid, and further comprises the following steps:
s1: opening a first valve 5 and a seventh valve 11, and injecting acetic acid waste liquid containing iodine simple substance into the membrane tube filter 1;
s2: the sixth valve 10 is opened, so that the clear liquid filtered by the membrane tube filter 1 is discharged from the clear liquid outlet tube 13 and can directly enter the subsequent treatment process of the acetic acid waste liquid;
s3: filtering the acetic acid waste liquid by a membrane tube filter 1 to form concentrated solution, and when the iodine simple substance in the concentrated solution is 10-20 times of the initial concentration, allowing the concentrated solution to enter a concentrated solution storage tank 3; in this embodiment, the concentration of elemental iodine in the waste liquid entering the concentrate tank 3 is preferably 10 times the initial concentration.
S4: after the amount of the concentrated solution collected in the concentrated solution storage tank 3 meets the separation amount of the centrifuge, opening a fourth valve 8 to inject the concentrated solution into the centrifuge 4; in this embodiment, the concentrate tank 3 is filled with concentrate and then the fourth valve 8 is opened to perform centrifugal separation.
S5: separating iodine simple substance from the concentrated solution after centrifugation by a centrifugal machine 4, and forming centrifugal clear liquid; after separation is completed, the centrifugal machine is stopped 4, a fifth valve 9 on a solid outlet pipe is opened, iodine simple substances are filled into a collecting bag, meanwhile, a third valve 7 is opened, and centrifugal clear liquid is injected into the membrane tube filter 1 through a liquid return pipe 16.
Further, the method further comprises the step of back flushing, wherein when the membrane tube filter 1 is used for filtering, a differential pressure gauge is used for detecting the differential pressure of the front end and the rear end of the membrane tube filter 1, when the differential pressure of the front end and the rear end of the membrane tube filter 1 reaches 50-150 kPa, back flushing operation is carried out, at the moment, the fourth valve 8, the sixth valve 10 and the seventh valve 11 are closed, the second valve 6 is opened, flushing fluid in the back flushing water tank 2 enters the membrane tube filter 1 through the back flushing pipe 17 to back flush the membrane tube filter 1, the flow of desalted water in each back flushing is 3-5 times the feeding flow of the membrane tube filter 1, the time of each back flushing operation is 5-10 min, preferably 10min, the second valve 6 is closed, the fourth valve 8, the sixth valve 10 and the seventh valve 11 are opened, and solid-liquid separation operation is continued.
While the foregoing is directed to the preferred embodiment of the present utility model, other and further embodiments of the utility model may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. The technical scope of the present utility model is not limited to the description, but must be determined according to the scope of claims.

Claims (6)

1. A solid-liquid separation system of iodine-containing acetic acid waste liquid is characterized in that: the device comprises a membrane tube filter, a concentrated solution storage tank and a centrifuge, wherein the membrane tube filter is provided with a waste liquid inlet, a clear liquid outlet and a concentrated solution outlet, the waste liquid inlet is provided with a waste liquid inlet pipe for introducing iodine-containing acetic acid waste liquid, the waste liquid inlet pipe is provided with a first valve, the clear liquid outlet is provided with a clear liquid outlet pipe for leading out acetic acid solution after filtering iodine, the concentrated solution outlet is provided with a concentrated solution first outlet pipe, the other end of the concentrated solution first outlet pipe is connected to a liquid inlet of the concentrated solution storage tank, a liquid outlet of the concentrated solution storage tank is connected to a liquid inlet of the centrifuge through a concentrated solution second outlet pipe, and the concentrated solution second outlet pipe is provided with a fourth valve; the centrifugal machine is also provided with a solid outlet and a liquid return port for discharging solid iodine, and the solid outlet is used for discharging solid iodine simple substances separated by the centrifugal machine; the liquid return port is provided with a liquid return pipe, the other end of the liquid return pipe is connected to the waste liquid inlet pipe, and the liquid return pipe is provided with a third valve.
2. The solid-liquid separation system of the iodine-containing acetic acid waste liquid according to claim 1, wherein: the device further comprises a sixth valve and a seventh valve, wherein the sixth valve is arranged on the clear liquid outlet pipe, the seventh valve is arranged on the waste liquid inlet pipe between the first valve and the waste liquid inlet, the sixth valve is used for controlling the flow rate of the clear liquid outlet, and the seventh valve is used for controlling the flow rate of the waste liquid inlet.
3. The solid-liquid separation system of the iodine-containing acetic acid waste liquid according to claim 2, wherein: the ratio of the flow of the clear liquid outlet to the flow of the waste liquid inlet is controlled to be 0.7-0.9.
4. The solid-liquid separation system of the iodine-containing acetic acid waste liquid according to claim 1, wherein: the membrane tube filter is characterized by further comprising a differential pressure gauge and a back flushing water tank, wherein the differential pressure gauge is connected in parallel with the two ends of an inlet and an outlet of the membrane tube filter and used for detecting the differential pressure of the front end and the rear end of the membrane tube filter, the membrane tube filter is further provided with a back flushing liquid inlet, the back flushing water tank is connected to the back flushing liquid inlet of the membrane tube filter through a back flushing tube, and a second valve is arranged on a pipeline between the back flushing water tank and the back flushing liquid inlet.
5. The solid-liquid separation system of the iodine-containing acetic acid waste liquid according to claim 1, wherein: the membrane tube in the membrane tube filter is made of ceramics, siC or Al 2 O 3
6. The solid-liquid separation system of the iodine-containing acetic acid waste liquid according to claim 1, wherein: the device also comprises a control unit, wherein the control unit is connected with each valve in the solid-liquid separation system through a circuit so as to realize automatic control.
CN202321003629.2U 2023-04-28 2023-04-28 Solid-liquid separation system of iodine-containing acetic acid waste liquid Active CN220245678U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202321003629.2U CN220245678U (en) 2023-04-28 2023-04-28 Solid-liquid separation system of iodine-containing acetic acid waste liquid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202321003629.2U CN220245678U (en) 2023-04-28 2023-04-28 Solid-liquid separation system of iodine-containing acetic acid waste liquid

Publications (1)

Publication Number Publication Date
CN220245678U true CN220245678U (en) 2023-12-26

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN202321003629.2U Active CN220245678U (en) 2023-04-28 2023-04-28 Solid-liquid separation system of iodine-containing acetic acid waste liquid

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