CN113908889A - Ion exchange resin transformation regeneration method and batch processing device - Google Patents

Ion exchange resin transformation regeneration method and batch processing device Download PDF

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Publication number
CN113908889A
CN113908889A CN202111381699.7A CN202111381699A CN113908889A CN 113908889 A CN113908889 A CN 113908889A CN 202111381699 A CN202111381699 A CN 202111381699A CN 113908889 A CN113908889 A CN 113908889A
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resin
solution
regeneration
transformation
ion exchange
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刘雨程
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Xian Thermal Power Research Institute Co Ltd
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Xian Thermal Power Research Institute Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J49/00Regeneration or reactivation of ion-exchangers; Apparatus therefor
    • B01J49/60Cleaning or rinsing ion-exchange beds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J49/00Regeneration or reactivation of ion-exchangers; Apparatus therefor
    • B01J49/80Automatic regeneration
    • B01J49/85Controlling or regulating devices therefor
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/44Resins; Plastics; Rubber; Leather
    • G01N33/442Resins; Plastics

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Food Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Treatment Of Water By Ion Exchange (AREA)

Abstract

The ion exchange resin transferring and regenerating method includes soaking and washing ion exchange resin with transferring and regenerating medicine to complete the transfer of resin with different ions, unified ion form and stable resin state. The invention also discloses an ion exchange resin batch processing device, which consists of a transformation regeneration medicament storage module, a control module, a dosing module and a resin storage module. When the device is used, the drug adding module is used for conveying the drugs to the resin storage module and reacting with the resin, and the control module automatically adjusts parameters such as the type, the drug adding amount, the drug adding sequence and the like of the transformation regeneration drugs according to the difference of the resin types. The invention realizes the batch, automation and intellectualization of the transformation regeneration of the ion exchange resin and improves the transformation regeneration efficiency of the ion exchange resin.

Description

Ion exchange resin transformation regeneration method and batch processing device
Technical Field
The invention belongs to the technical field of ion exchange resin detection, and particularly relates to an ion exchange resin transformation regeneration method and a batch processing device.
Background
Ion exchange resins are widely applied to the fields of chemical industry, pharmacy, water treatment and the like, so that the performance of the ion exchange resins is detected, and the quality determination, the service life diagnosis and the like of the resins are involved.
The ion exchange resin exchanges with the ion in the solution through the exchangeable ion on the macromolecular skeleton of the ion exchange resin, so as to remove the ion in the solution. In actual use, the types of exchangeable ions on the framework of the ion exchange resin are different, the state of the resin is unknown, the ion form is difficult to determine, and the resin needs to be repeatedly transformed before performance test or use of the resin, so that all the resins are ensured to be in a uniform ion form and a stable state. Meanwhile, after a period of use of the ion exchange resin, exchangeable ions thereof are replaced by ions in the solution, resulting in failure of the resin. At this time, the resin must be regenerated by transformation to have ion exchange capacity again, and the resin can be used continuously. If the transformation or regeneration of the ion exchange resin is not thorough, the performance judgment and use of the ion exchange resin are seriously influenced.
Disclosure of Invention
The invention aims to provide an ion exchange resin transformation regeneration method and a batch processing device with good transformation regeneration effect, thorough transformation and good reproducibility, namely, aiming at different types of ion exchange resins, the effect of the transformation regeneration of the ion exchange resins is achieved through soaking and scouring of different types and sequences of transformation regeneration medicaments.
In order to achieve the purpose, the invention adopts the following technical scheme:
an ion exchange resin transformation regeneration method comprises the following steps:
step 1: measuring 30-50 mL of resin to an exchange column with a piston below;
step 2: soaking and washing the resin by using deionized water with the volume being 18-22 times that of the resin to remove impurities on the surface of the resin;
and step 3: soaking and washing the resin by using a transformation medicament with the volume 18-22 times that of the resin, so that the resin is transformed thoroughly and is stable in state;
and 4, step 4: soaking and washing the resin by using deionized water with the volume being 18-22 times that of the resin, and removing a transformation agent in the resin;
and 5: soaking and washing the resin by using a regeneration agent with the volume 28-32 times that of the resin to stabilize the state of the resin and completely regenerate the resin into a target ion form;
step 6: soaking and washing the resin by deionized water until no regenerative medicament exists in the system;
if the treated resin is difficult to transform and regenerate, the steps 2 to 5 are repeated for a plurality of times before the step 6 is carried out.
The transformation reagent is a solution which does not carry ions with the same form as the target ions of the resin, and the solution can elute the target ions on the resin to ensure that the resin is invalid; the solution is acid solution, alkali solution or salt solution, and the concentration is 1 mol/L.
The regeneration agent is a solution carrying ions with the same form as the target ions of the resin, and the solution can enable the resin to carry the target ions to complete resin regeneration; the solution is acid solution, alkali solution or salt solution, and the concentration is 1 mol/L.
The flow rates of the transformation medicament, the regeneration medicament and the deionized water are 10 mL/min.
The liquid level of the rotary agent, the regenerative agent or the deionized water in the exchange column is always higher than the top end of the resin layer by 1-2 cm.
The batch processing device for realizing the ion exchange resin transformation regeneration method comprises a transformation regeneration medicament storage module A, a dosing module C, a control module B and a resin storage module D, wherein the modules are connected by a corrosion-resistant pipeline;
the transformation regeneration medicament storage module A consists of a series of corrosion-resistant containers A1 which are respectively filled with transformation medicaments, regeneration medicaments and deionized water, the number of the containers A1 is increased or decreased according to the specific resin types, and the outlet of the container A1 is connected with the inlet of the multi-channel switching valve through a corrosion-resistant pipeline;
the control module B consists of a controller B2 and a multi-channel switching valve B1;
the medicine adding module C consists of a pump C1 and a pipeline, and solution in the transformation regeneration medicine storage module is led to an exchange column of the resin storage module through a multi-channel switching valve B1;
the resin storage module D is an exchange column with a hole partition plate 1, a tee joint 2 is connected to an outlet of the exchange column, one end of the tee joint is connected with a U-shaped pipe 4, the outlet of the U-shaped pipe 4 is 1-2 cm higher than the top end of the resin layer in the treatment process, the liquid level height in the resin storage module is kept through atmospheric pressure, and the situation that the liquid level of rotary reagents, regenerative reagents and deionized water in the exchange column is lower than the resin layer to cause insufficient treatment is avoided; and the other end of the tee joint is provided with an electromagnetic valve 3 for emptying the medicament in the exchange column, and the electromagnetic valve is controlled by a controller B2 of the control module B.
The device can be expanded in parallel, and different types of ion exchange resins can be transformed and regenerated in batches at the same time through the control module.
Compared with the prior art, the invention has the following advantages:
1. the invention provides a method for transforming and regenerating ion exchange resin, which can transform brand-new resin with non-uniform ion form and used resin with changed ion form into target form and stabilize the resin state.
2. The ion exchange resin transformation regeneration method provided by the invention can adjust parameters such as the type, the dosage, the dosing sequence and the like of transformation regeneration medicaments, thereby meeting the requirements of different types of resins on transformation regeneration.
3. The ion exchange resin transformation regeneration method provided by the invention has reasonable dosage and variety of transformation regeneration agents and has good transformation regeneration effect on different types of resins.
4. The ion exchange resin transformation regeneration method provided by the invention has stable transformation regeneration effect and good reproducibility, and can reduce result fluctuation caused by different operation habits of personnel.
5. The ion exchange resin transformation regeneration batch processing device provided by the invention can automatically maintain the liquid level of deionized water or treatment agent in the exchange column, and avoid incomplete transformation regeneration caused by the fact that the liquid level of the deionized water or transformation regeneration agent is lower than the resin layer.
6. The invention provides an ion exchange resin transformation regeneration batch processing device, which can simultaneously carry out transformation regeneration operation on a plurality of groups of different types of resins, greatly reduce the workload of the transformation regeneration of the ion exchange resin, improve the transformation regeneration efficiency, and simultaneously avoid the influence on the transformation regeneration effect of the ion exchange resin due to human misoperation.
Drawings
FIG. 1 is a schematic view of an ion exchange resin batch processing apparatus according to the present invention;
FIG. 2 is a schematic view of a resin storage module in the batch processing apparatus for ion exchange resin amount according to the present invention;
FIG. 3 shows the results of a full exchange capacity test of ion exchange resins treated by manual treatment and the apparatus of the present invention, respectively.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
The ion exchange resin conversion regeneration method of the invention uses corresponding conversion regeneration medicament to wash the resin according to the different types of the resin, so as to lead the ion types carried by the resin to be uniform and the state to be stable. In the case of a sodium type strongly acidic cation exchange resin, sodium ions carried by the resin may be replaced by hydrogen ions, etc., and in order to accurately test or use the resin, transformation regeneration is performed, and the hydrogen ions are replaced by the sodium ions, etc.
To more intuitively explain the method for transforming and regenerating an ion exchange resin according to the present invention, a sodium type strongly acidic cation exchange resin (model number D001 MBP) is taken as an example, and the specific embodiment thereof will be described in detail. The present invention should not be construed as being limited to only the conversion regeneration of the resin.
1. Adding 30mL of ion exchange resin into an exchange column with a piston at the lower part;
2. closing a piston below the exchange column, and adding deionized water into the exchange column to enable the liquid level to be 1-2 cm higher than the upper end of the resin layer;
3. adding 600mL of deionized water into the exchange column through a separating funnel at the flow rate of 10mL/min, and adjusting a piston below the exchange column to enable the liquid level in the column to be 1-2 cm higher than the upper end of the resin layer all the time;
4. adding 600mL of HCl solution into the exchange column through a separating funnel at the flow rate of 10mL/min, and adjusting a piston below the exchange column to enable the liquid level in the column to be 1-2 cm higher than the upper end of the resin layer all the time;
5. adding 600mL of deionized water into the exchange column through a separating funnel at the flow rate of 10mL/min, and adjusting a piston below the exchange column to enable the liquid level in the column to be 1-2 cm higher than the upper end of the resin layer all the time;
6. adding 900mL of NaCl solution into the exchange column through a separating funnel at the flow rate of 10mL/min, and adjusting a piston below the exchange column to enable the liquid level in the column to be 1-2 cm higher than the upper end of the resin layer all the time;
7. adding deionized water into the exchange column at a flow rate of 10mL/min through a separating funnel, and adjusting a piston below the exchange column to enable the liquid level in the column to be 1-2 cm higher than the upper end of the resin layer all the time until the effluent cannot enable AgNO3Until the solution became white.
So far, the exchangeable ions of the resin are all Na+And completing the transformation regeneration of the sodium type strong-acid cation exchange resin.
As shown in fig. 1, the ion exchange resin batch processing device of the present invention is composed of a transforming regenerative medicament storage module a, a dosing module C, a control module B and a resin storage module D, wherein each module is connected by a corrosion-resistant pipeline;
the transformation regeneration medicament storage module A consists of a series of corrosion-resistant containers A1 which are respectively filled with transformation medicaments, regeneration medicaments and deionized water, the number of the containers A1 is increased or decreased according to the specific resin types, and the outlet of the container A1 is connected with the inlet of the multi-channel switching valve through a corrosion-resistant pipeline;
the control module B consists of a controller B2 and a multi-channel switching valve B1;
the medicine adding module C consists of a pump C1 and a pipeline, and solution in the transformation regeneration medicine storage module is led to an exchange column of the resin storage module through a multi-channel switching valve B1;
as shown in fig. 2, the resin storage module D is an exchange column with a perforated partition plate 1, a tee joint 2 is connected to an outlet of the exchange column, one end of the tee joint is connected to a U-shaped pipe 4, and the outlet of the U-shaped pipe 4 should be 1-2 cm higher than the top end of the resin layer in the treatment process, the liquid level in the resin storage module is maintained by atmospheric pressure, and the situation that the liquid level of the rotary reagent, the regenerative reagent and the deionized water in the exchange column is lower than the resin layer, which results in insufficient treatment, is prevented; and the other end of the tee joint is provided with an electromagnetic valve 3 for emptying the medicament in the exchange column, and the electromagnetic valve is controlled by a controller B2 of the control module B.
To more intuitively explain the operation of the batch processing apparatus for ion exchange resin according to the present invention, a sodium type strongly acidic cation exchange resin (model number D001 MBP) is taken as an example, and the detailed description will be given. However, the present invention is not limited to the transformation regeneration of the resin.
1. Respectively adding sufficient NaOH solution, sufficient HCl solution and sufficient deionized water into each container A1 of the transformation regeneration medicament storage module A;
2. adding 30mL of sodium type strong-acid cation exchange resin and deionized water into the resin storage module D, and adjusting the height of the U-shaped tube to enable the liquid level of the deionized water in the exchange column to be 1-2 cm higher than the upper end of the resin layer;
3. opening a power supply of the dosing module and the control module, and loading a control instruction of conversion regeneration of the sodium type strong-acid cation exchange resin;
4. the dosing module C adds 600mL of deionized water into the resin storage module D at the flow rate of 10mL/min, flows out of the resin storage module D through the U-shaped pipe 4, and removes impurities on the surface of the resin through flushing of the deionized water.
5. The drug adding module C adds 600mL of HCl solution into the resin storage module D at the flow rate of 10mL/min, flows out of the resin storage module D through the U-shaped pipe 4, and converts ions carried by the resin into H through the flushing of the HCl solution+
6. Controller B2 purged the HCl solution from the column through solenoid valve 3. The dosing module C adds 600mL of deionized water into the resin storage module D at the flow rate of 10mL/min, flows out of the resin storage module D through the U-shaped pipe 4, and washes away the residual HCl solution in the device through the deionized water.
7. The medicine adding module C adds 900mL of NaCl solution into the resin storage module D at the flow rate of 10mL/min, the NaCl solution flows out of the resin storage module D through the U-shaped pipe, and ions carried by the resin are converted into Na through the flushing of the NaCl solution+
8. The controller B2 discharges the NaCl solution in the exchange column through the electromagnetic valve 3. And the dosing module C adds deionized water into the resin storage module D at the flow rate of 10mL/min, flows out of the resin storage module D through the U-shaped pipe 4, and washes the residual NaCl solution in the device through the deionized water. 5mL of effluent liquid is taken every 10min and added with silver nitrate indicating liquid, and the water washing is stopped until no white precipitate is generated.
So far, the exchangeable ions of the resin are all Na+And completing the transformation regeneration of the sodium type strong-acid cation exchange resin.
The treatment steps are repeated on the same batch of resin samples, then the total exchange capacity of the samples after two times of treatment is respectively tested and compared with the samples treated manually, and the results show that the treatment device has no difference between the transformation regeneration effect of the ion exchange resin and the manual operation, the repeatability and the consistency are good, and the treated resin is stable in state and consistent in form.
Further, after different types of ion exchange resins were treated by manual treatment and the treatment device, the exchange capacities were measured, and the results are shown in fig. 3, which shows that the results of the total exchange capacity test were consistent. Compared with manual operation, the ion exchange tree batch processing device provided by the invention is used for carrying out transformation regeneration operation on resin, has high processing efficiency, is not easy to make mistakes, and has the same result as a manual operation result.

Claims (8)

1. The method for transforming and regenerating the ion exchange resin is characterized by comprising the following steps of:
step 1: measuring 30-50 mL of resin to an exchange column with a piston below;
step 2: soaking and washing the resin by using deionized water with the volume being 18-22 times that of the resin to remove impurities on the surface of the resin;
and step 3: soaking and washing the resin by using a transformation medicament with the volume 18-22 times that of the resin, so that the resin is transformed thoroughly and is stable in state;
and 4, step 4: soaking and washing the resin by using deionized water with the volume being 18-22 times that of the resin, and removing a transformation agent in the resin;
and 5: soaking and washing the resin by using a regeneration agent with the volume 28-32 times that of the resin to stabilize the state of the resin and completely regenerate the resin into a target ion form;
step 6: and soaking and washing the resin by deionized water until no regenerative medicament exists in the system.
2. The method of claim 1, wherein step 2-step 5 are repeated several times before step 6 if the treated resin is difficult to transform and regenerate.
3. The method of claim 1, wherein the transforming agent is a solution that does not carry ions of the same form as the target ions of the resin, and the solution elutes the target ions from the resin, rendering the resin ineffective; the solution is acid solution, alkali solution or salt solution, and the concentration is 1 mol/L.
4. The method of claim 1, wherein the regenerating agent is a solution carrying ions of the same form as the target ions of the resin, and the solution can make the resin carry the target ions to complete the regeneration of the resin; the solution is acid solution, alkali solution or salt solution, and the concentration is 1 mol/L.
5. The method of claim 1, wherein the flow rates of the transforming agent, the regenerating agent and the deionized water are 10 mL/min.
6. The method of claim 1, wherein the liquid level of the transfer agent, the regeneration agent or the deionized water in the column is always 1-2 cm higher than the top of the resin layer.
7. The batch processing device for realizing the ion exchange resin transformation regeneration method according to claim 1, which is characterized by consisting of a transformation regeneration medicament storage module (A), a dosing module (C), a control module (B) and a resin storage module (D), wherein the modules are connected by corrosion-resistant pipelines;
the transformation regeneration medicament storage module (A) consists of a series of corrosion-resistant containers (A1) which are respectively filled with transformation medicaments, regeneration medicaments and deionized water, the number of the containers (A1) is increased or decreased according to the specific resin types, and the outlet of the container (A1) is connected with the inlet of the multi-channel switching valve through a corrosion-resistant pipeline;
the control module (B) consists of a controller (B2) and a multi-channel switching valve (B1);
the medicine adding module (C) consists of a pump (C1) and a pipeline, and the solution in the transformation regeneration medicine storage module is led to the exchange column of the resin storage module through a multi-channel switching valve (B1);
the resin storage module (D) is an exchange column with a hole partition plate (1), a tee joint (2) is connected to the outlet of the exchange column, one end of the tee joint is connected with a U-shaped pipe (4), the outlet of the U-shaped pipe (4) is 1-2 cm higher than the top end of the resin layer in the treatment process, the liquid level in the resin storage module is maintained through atmospheric pressure, and the situation that the liquid level of rotary reagents, regenerative reagents and deionized water in the exchange column is lower than the resin layer to cause insufficient treatment is prevented; the other end of the tee joint is provided with an electromagnetic valve (3) for emptying the medicament in the exchange column, and the electromagnetic valve is controlled by a controller (B2) of the control module (B).
8. The batch processing device according to claim 7, wherein the device is developed in parallel, and different types of ion exchange resins are simultaneously transformed and regenerated in batches through the control module.
CN202111381699.7A 2021-11-22 2021-11-22 Ion exchange resin transformation regeneration method and batch processing device Pending CN113908889A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR970058779A (en) * 1996-01-25 1997-08-12 이규철 Ion exchange resin transfer separation regeneration method and apparatus of out-of-phase regenerative mixed-phase multiple desalination plant
CN201431886Y (en) * 2009-06-16 2010-03-31 上海轻工业研究所有限公司 Batch regeneration device of ion exchange resin
CN102659568A (en) * 2012-05-03 2012-09-12 中粮生物化学(安徽)股份有限公司 Method for continuously removing cations out of solution containing citric acid
CN103769249A (en) * 2012-10-25 2014-05-07 中国石油化工股份有限公司 Ion exchange method
CN205627987U (en) * 2016-05-23 2016-10-12 华电内蒙古能源有限公司包头发电分公司 Cation exchange resin's dynamic regenerating unit discolours
CN106282560A (en) * 2016-04-28 2017-01-04 南京霖厚环保科技有限公司 In acid solution containing nickel, the extraction and cleaning of nickel controls technique
CN106587433A (en) * 2016-12-20 2017-04-26 无锡出新环保设备有限公司 Chromium-containing waste water treatment system adopting double anion exchange columns and treatment method of system
CN207204125U (en) * 2017-09-15 2018-04-10 深圳市加美富实业有限公司 Resin column automatic regeneration device
CN107999149A (en) * 2017-12-14 2018-05-08 长沙理工大学 A kind of method for resuscitation and recovery medicament of the cation exchange resin of organic basifier pollution
CN113030347A (en) * 2021-04-26 2021-06-25 山东电力研究院 Pretreatment device and method for determining soluble salt components based on ion chromatography
CN113042114A (en) * 2021-04-28 2021-06-29 武汉恩孚水务有限公司 Ion exchange resin regeneration process and device
CN216419429U (en) * 2021-11-22 2022-05-03 西安热工研究院有限公司 Ion exchange resin transformation regeneration batch processing device

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR970058779A (en) * 1996-01-25 1997-08-12 이규철 Ion exchange resin transfer separation regeneration method and apparatus of out-of-phase regenerative mixed-phase multiple desalination plant
CN201431886Y (en) * 2009-06-16 2010-03-31 上海轻工业研究所有限公司 Batch regeneration device of ion exchange resin
CN102659568A (en) * 2012-05-03 2012-09-12 中粮生物化学(安徽)股份有限公司 Method for continuously removing cations out of solution containing citric acid
CN103769249A (en) * 2012-10-25 2014-05-07 中国石油化工股份有限公司 Ion exchange method
CN106282560A (en) * 2016-04-28 2017-01-04 南京霖厚环保科技有限公司 In acid solution containing nickel, the extraction and cleaning of nickel controls technique
CN205627987U (en) * 2016-05-23 2016-10-12 华电内蒙古能源有限公司包头发电分公司 Cation exchange resin's dynamic regenerating unit discolours
CN106587433A (en) * 2016-12-20 2017-04-26 无锡出新环保设备有限公司 Chromium-containing waste water treatment system adopting double anion exchange columns and treatment method of system
CN207204125U (en) * 2017-09-15 2018-04-10 深圳市加美富实业有限公司 Resin column automatic regeneration device
CN107999149A (en) * 2017-12-14 2018-05-08 长沙理工大学 A kind of method for resuscitation and recovery medicament of the cation exchange resin of organic basifier pollution
CN113030347A (en) * 2021-04-26 2021-06-25 山东电力研究院 Pretreatment device and method for determining soluble salt components based on ion chromatography
CN113042114A (en) * 2021-04-28 2021-06-29 武汉恩孚水务有限公司 Ion exchange resin regeneration process and device
CN216419429U (en) * 2021-11-22 2022-05-03 西安热工研究院有限公司 Ion exchange resin transformation regeneration batch processing device

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