CN113198550A - Method for off-line regeneration of ion exchange resin in situ - Google Patents
Method for off-line regeneration of ion exchange resin in situ Download PDFInfo
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- CN113198550A CN113198550A CN202110505695.9A CN202110505695A CN113198550A CN 113198550 A CN113198550 A CN 113198550A CN 202110505695 A CN202110505695 A CN 202110505695A CN 113198550 A CN113198550 A CN 113198550A
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
- B01J49/50—Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
- B01J49/50—Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents
- B01J49/53—Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents for cationic exchangers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
- B01J49/50—Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents
- B01J49/57—Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents for anionic exchangers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
The invention relates to a method for off-line regeneration of ion exchange resin in situ, which is characterized in that a movable combined off-line resin regeneration device is arranged on a resin user site to regenerate the resin which is failed by the resin user; the method comprises the steps of backwashing and separating the failed resin by using nitrogen and filtered water provided by a resin user; and regenerating the resin by adopting the medicine and the ultrapure water provided by the resin user. The method effectively reduces the risk of resin pollution, can also improve the regeneration quality of the resin, improve the effluent quality and effectively shorten the regeneration and delivery period.
Description
Technical Field
The invention belongs to the technical field of water treatment, and particularly relates to a method for in-situ off-line regeneration of ion exchange resin, in particular to in-situ off-line regeneration of polishing mixed bed resin.
Background
The ion exchange system is a water treatment process for replacing various anions and cations in water by anion and cation exchange resins, the anion and cation exchange resins are matched singly or in different proportions to form an ion exchange cation bed system, an ion exchange anion bed system and an ion exchange mixed bed system, and the mixed bed system is a terminal process which is usually used for preparing ultrapure water and high-purity water after water treatment processes such as reverse osmosis and the like, and is one of irreplaceable means for preparing the ultrapure water and the high-purity water. The mixed bed is a system which mixes and fills cation and anion exchange resin in a certain proportion in the same exchange device. Various mineral salts in water can be substantially removed by the mixed bed, and the mixed bed is widely applied to the preparation of ultrapure water and high-purity water in the ultrapure industry for industries such as semiconductor electronics, liquid crystal industry and the like.
As the use time is prolonged, the cation resin and the anion resin are saturated, so that the capacity of replacing ions in water is lost, and the resin needs to be replaced regularly. The method of purchasing and replacing new resin can be adopted, but the delivery time of the new resin is long, the time of 1 year is usually needed at present, the price of a resin manufacturer is increased, the cost is increased year by year, and in addition, the environmental load is increased and the resource waste is caused because old resin is discarded. If the resin regeneration mode is adopted, the continuous regeneration and utilization of the resin can be realized, the delivery time can be greatly shortened, and the operation cost can be effectively reduced.
Regeneration of ion exchange mixed bed systems can now be divided into in vivo synchronous regeneration (also known as on-line regeneration) and in vitro regeneration (also known as off-line regeneration). The whole regeneration process of in vivo synchronous regeneration is carried out in a mixed bed, firstly injecting HCL (hydrogen chloride) into a column body, converting positive resin into H type, then washing, then injecting NaOH (sodium hydroxide), converting negative resin into OH type, then washing, and needing pH value to be neutral. The resin is not moved out of the device during regeneration, and the male resin and the female resin are regenerated simultaneously, so that the required accessory devices are few, and the arrangement is centralized. The defects are that the regeneration operation steps are complex, the time consumption is long, the regeneration effect is unstable, the requirement on the operation skill of workers is high, and the regeneration waste liquid is easy to pollute the resin and the like.
The in vitro regeneration has the advantages of simple regeneration operation steps, good regeneration effect, resin pollution prevention and the like, but the existing in vitro regeneration type mixed bed has more accessory facilities, needs to be provided with related equipment such as a resin storage tower and the like, and increases the manufacturing cost of the equipment. In the existing in-vitro regeneration, special in-vitro regeneration equipment is arranged in a resin factory, the failed resin is taken out at a client site and transported to the resin factory for regeneration, and the regenerated resin is transported to the client site for mixing and using. The resin is transported back and forth in the process, the period is long, and the resin pollution risk is high in the transfer process; pure water is adopted in a resin factory, and micro-particles and trace metals are unstable and influence on the regeneration effect of the resin; the anion and cation resins are not mixed in a resin factory and return to a customer site for mixing, and the quality of the final effluent cannot be detected; in addition, the resin is complex to store and manage, the risk of mixing resin of different users and different brands is high, acid-base waste liquid is generated by resin regeneration, and the resin needs to be treated separately, so that the cost is high. Therefore, how to comprehensively solve the problems is worthy of further study.
Disclosure of Invention
Problems to be solved by the invention
In order to solve the above technical problems, the present invention aims to provide a method for performing off-line regeneration of ion exchange resin on site, which effectively reduces the risk of resin pollution, and can also improve the regeneration quality of resin, improve the effluent quality, and effectively shorten the regeneration and delivery cycle.
Means for solving the problems
The invention comprises the following technical scheme:
[1] a method for carrying out the off-line regeneration of ion exchange resin on site, wherein,
the method is that the movable combined resin off-line regeneration device is arranged on a resin user site to regenerate the resin which is failed by the resin user;
the device mainly comprises: the resin separation assembly, the positive resin regeneration assembly, the negative resin regeneration assembly and the resin mixing and detecting assembly;
the method comprises the steps of backwashing and separating the failed resin in the resin separation assembly by using nitrogen and filtered water provided by the resin user; and regenerating the resin in the positive resin regeneration assembly and the negative resin regeneration assembly by adopting the medicine and the ultrapure water provided by the resin user.
[2] The method according to [1], wherein the resin off-line regeneration apparatus further comprises a plurality of holders by which the resin separation module, the male resin regeneration module, the female resin regeneration module, and the resin mixture detection module are assembled together in a detachable manner from each other.
[3] The method according to [1] or [2], wherein the resin separation module comprises a resin input device and a separation column, and the resin mixing and detecting module comprises a male metering tank, a female metering tank, a mixing tank, and a resin detecting device.
[4] The method according to [3], wherein the male resin regeneration module comprises a male half tank, a male conversion tower and a male resin tank, and the female resin regeneration module comprises a female half tank, a female conversion tower, a female resin tank and a heat exchanger. [5] The method according to [3] or [4], further comprising transferring the male resin and the female resin separated by the separation tower to a male semi-finished product tank and a female semi-finished product tank for temporary storage respectively; and respectively detecting the mixing rate of the positive resin and the negative resin before transferring to the positive semi-finished product groove and the negative semi-finished product groove.
[6] The method according to any one of the items [3] to [5], wherein the method further comprises transferring the regenerated male resin and the regenerated female resin to a male resin tank and a female resin tank respectively by using nitrogen and ultrapure water supplied by the resin user after the regeneration is finished, and transferring the male resin and the regenerated female resin to the male metering tank and the female metering tank respectively for precise metering before the resins enter the mixing tank.
[7] The method according to [6], further comprising metering, charging into a mixing tank in the order of yin first and yang second, and washing the resins in the mixing tank and mixing them thoroughly.
[8]According to [1]～[7]The method of any of the above aspects, wherein the method further comprises sampling the mixed resin to a resin detection device to determine the total organic carbon content, resistivity, particulates, and SiO of the effluent2Content and/or ion content analysis.
[9] The method according to any one of [1] to [8], wherein the resin user supplies ultrapure water having a resistivity of >18M Ω & cm and TOC <30 ppb.
[10] The method according to any one of [1] to [9], wherein the resin is a polished mixed bed resin used for an ultrapure water system.
ADVANTAGEOUS EFFECTS OF INVENTION
The method for off-line regeneration of the ion exchange resin on site provided by the invention has the advantages that the resin does not need to be transported, can be regenerated on site after being taken out from the existing mixed bed system of a user, and can be put into use immediately after being regenerated, so that the possibility of pollution of the resin is reduced, and the regeneration and delivery cycle is effectively shortened. Moreover, because the resins are all the resins of the same user, the resin mixing phenomenon of different manufacturers can not occur, and the management is convenient. In addition, the method fully utilizes the existing equipment and medicines of a user site, can improve the regeneration quality of the resin, and effectively reduces the production cost.
The method of the invention adopts the skid-mounted movable combined resin off-line regeneration device, can effectively reduce the floor area, can be flexibly arranged according to the actual field conditions of different fields, and has simple and convenient piping and convenient assembly and disassembly.
In some embodiments of the invention, the resin off-line regeneration device with a specific structure is adopted, and the regeneration, mixing and detection steps are adjusted, optimized and detected, so that the accuracy of the proportion mixing ratio of the resin is high, the regeneration quality of the resin is further improved, and in addition, after the resin is mixed, the TOC and the resistivity of the inlet water and the outlet water are sampled and measured, and the quality of the mixed outlet water is further ensured.
The above description does not disclose all embodiments of the present invention and all advantages of the present invention.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. The drawings in the following description are some embodiments of the invention, and it is obvious to those skilled in the art that other drawings can be obtained from the drawings without inventive effort.
Fig. 1 is a plan view schematically illustrating a resin off-line recycling apparatus according to a first embodiment of the present invention.
Fig. 2 is a schematic view of a piping arrangement of the resin off-line regeneration apparatus according to the first embodiment of the present invention.
Reference numerals
11-resin feeding device
12-separation column
13-yang semi-finished product groove
14-tank for female semi-finished products
15-sun conversion tower
16-negative conversion tower
17-Positive resin tank
18-negative resin tank
19-positive metering tank
20-negative measuring tank
21-mixing tank
22-resin detection device
23-Heat exchanger
Detailed Description
In the following detailed description, numerous specific details are set forth in order to provide a better understanding of the invention. It will be understood by those skilled in the art that the present invention may be practiced without some of these specific details. In other instances, methods, means, devices and steps which are well known to those skilled in the art have not been described in detail so as not to obscure the invention.
Unless defined otherwise, technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
In the present specification, the numerical range represented by "numerical value a to numerical value B" means a range including the end point numerical value A, B. In the present specification, the meaning of "may" includes both the meaning of performing a certain process and the meaning of not performing a certain process. In this specification, "optional" or "optionally" means that the subsequently described event or circumstance may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
In the present specification, references to "some specific/preferred embodiments," "other specific/preferred embodiments," "technical solutions," "embodiments," and the like, mean that a particular element (e.g., feature, structure, property, and/or characteristic) described in connection with the embodiment is included in at least one embodiment described herein, and may or may not be present in other embodiments. In addition, it is to be understood that the described elements may be combined in any suitable manner in the various embodiments.
The terms "comprises" and "comprising," and any variations thereof, in the description and claims of this invention and the above-described drawings are intended to cover non-exclusive inclusions. For example, a process, method, or system, article, or apparatus that comprises a list of steps or elements is not limited to only those steps or elements listed, but may alternatively include other steps or elements not listed, or inherent to such process, method, article, or apparatus.
The resin user in the invention refers to a user using resin, for example, an electronic industry needing ultrapure water, such as a semiconductor and liquid crystal enterprise, and a polishing mixed bed resin system is used at an ultrapure water and high-purity water terminal, and the user fails to polish the resin after using the resin for a certain time, so that the resin needs to be regenerated.
The polishing mixed bed resin can also be called polishing resin for short, is generally used at the tail end of an ultrapure water treatment system to ensure that the water quality of the outlet water of the system can maintain the water use standard, the water quality of the outlet water can reach more than 18 megaohms, TOC and SiO2Has certain control capability. The ion type of the polishing resin is H, OH type, and the polishing resin can be used after being filled and is generally used in the semiconductor industry. The polishing mixed bed resin or polishing resin is formed by mixing H-type cation exchange resin and OH-type anion exchange resin.
The "component" in the present invention refers to a certain device, component or a combination of certain devices and components, which are divided according to functions, and the components may be combined together or separately arranged.
The invention is different from the conventional method for regenerating the ion exchange resin offline, in that the method adopts the method for regenerating the ion exchange resin offline on the site or in the spot of a resin user, and the method adopts a specific movable combined type resin offline regeneration device. The apparatus and the method for off-line regeneration of the ion exchange resin will be described in detail below.
< apparatus for regenerating resin off-line >
The off-line resin regeneration device is a movable combined type device, and the movable combined type device is a device which is convenient to install and move and has more than 2 modules. In some embodiments of the present invention, the off-line resin regenerating device of the present invention adopts a skid-mounted structure, and functional components are integrated on an integrated base, and the off-line resin regenerating device can be integrally mounted and moved in an integrated manner.
Further, the apparatus used in the present invention includes a plurality of holders by which the apparatus of the present invention is divided into a plurality of modules, which are assembled together in a manner detachable from each other. If all equipment is only placed in a module, the module can be difficult to move, even if universal wheels are arranged, the equipment is heavy and has no practical operability, and a single module has specific fixed requirements on the size of a place where the equipment is placed, so that the equipment cannot be placed and cannot be cleaned by users with limited available places. In some embodiments of the present invention, in view of easy movement and installation, a corresponding rack may be provided for each device to be fixed and supported, each device and rack constituting one module. According to the function, the simple and convenient piping and the convenient dismounting and the like, the modules are assembled into the components, in some specific embodiments of the invention, according to the function, the simple and convenient piping and the convenient dismounting and the like, the resin off-line regeneration device mainly comprises 4 components:
the resin separation assembly, the positive resin regeneration assembly, the negative resin regeneration assembly and the resin mixing and detecting assembly.
The resin separation assembly is used for separating the resin to be regenerated into the male resin and the female resin, the male resin regeneration assembly is used for regenerating the male resin, the female resin regeneration assembly is used for regenerating the female resin, and the resin mixing and detecting assembly is used for mixing the regenerated male resin and the regenerated female resin with each other and detecting the mixed resin.
In carrying out the method of the present invention, the resin separation module, the male resin regeneration module, the female resin regeneration module and the resin mixing and detecting module are installed and fixed on a horizontal installation surface. In a plan layout plan view of the resin off-line recycling apparatus, the resin separation module, the male resin recycling module, the female resin recycling module, and the resin mixing and detecting module are sequentially arranged along the first direction and occupy a rectangular region of a predetermined area. The pipe distribution parts of the 4 components are connected through flanges, and the steel structure parts are connected through bolts to form a complete resin off-line regeneration device, so that the whole resin regeneration process requirement is met.
The resin separation assembly comprises at least one resin input device for transporting and temporarily storing the spent resin to be regenerated, in some embodiments of the invention, the bottom of the resin input device can be provided with wheels to facilitate the transportation of the resin, and further, a wheeled trolley can be used as the resin input device, and the volume can be between 800 and 1500L. The resin separation assembly further comprises a separation tower, and the anion resin and the cation resin are separated in the separation tower. In some embodiments of the invention, a pneumatic diaphragm pump is used to transfer the spent resin from the resin dosing apparatus to the separation column. The separation tower can adopt conventional cylindrical separation tower equipment, the diameter is 1.5-2 m, and the height is 4-5 m.
The cation resin regeneration module comprises a cation intermediate product tank, a cation conversion tower and a cation resin tank, wherein one or more cation intermediate product tanks and one or more cation resin tanks are respectively arranged, the cation intermediate product tank is used for metering and cleaning the cation resin from the separation tower, and after cleaning, excessive liquid is discharged, and the cation resin regeneration module can be prepared by adopting common resin to obtain a polyethylene storage tank. The arrangement of the male semi-finished product groove is beneficial to the subsequent accurate control of the primary regeneration amount of the male converter, if the device is not arranged, the primary regeneration amount in the male converter is difficult to control, water exists in the converter, the metering is difficult, and the adverse effect on the mixed bed resin regeneration effect is caused by the poor control of the primary regeneration amount. In addition, if there is excess resin, it can be temporarily stored in the cation intermediate tank to wait for the next regeneration without affecting the use of the separation column and the cation exchange column. The positive conversion tower is used for regenerating the positive resin after washing from the positive semi-finished product tank. In some embodiments of the present invention, the positive resin is transferred from the positive semi-finished product tank to the positive conversion tower by using a pneumatic diaphragm pump, the positive conversion tower performs regeneration work, and after the regeneration is finished and cleaned, the regenerated positive resin is transferred to the positive resin tank for temporary storage by using nitrogen and ultrapure water provided by a user. The positive resin tank is used for storing regenerated positive resin from the positive converter, and can be prepared by using common resin to obtain a polyethylene storage tank. In some embodiments of the invention, the male half tank and the male resin tank have the same volume.
The female resin regeneration assembly comprises a female half product tank, a female conversion tower, a female resin tank and a heat exchanger, wherein one or more female half product tanks can be respectively arranged, the female half product tank is used for metering and cleaning the female resin from the separation tower, and excessive liquid is discharged after cleaning, the female half product tank and the female resin tank can be prepared by adopting common resin to obtain a polyethylene storage tank, for example, and the volume of the female half product tank is required to be larger than that of the male half product tank in consideration of the mixing ratio of mixed bed resin, and in some specific embodiments of the invention, the volume ratio of the male half product tank to the female half product tank is 1: 2-3. The arrangement of the female semi-finished product tank is beneficial to the primary regeneration amount of a subsequent female conversion tower to be accurately controlled, if the device is not arranged, the primary regeneration amount in the female conversion tower is difficult to control, water exists in the tower, metering is difficult, and the primary regeneration amount is not well controlled, so that the mixed bed resin regeneration effect is adversely affected. The negative conversion tower is used for regenerating the washed negative resin from the negative semi-finished product tank. In some embodiments of the present invention, the negative resin is transferred from the negative semi-product tank to the negative conversion tower by using a pneumatic diaphragm pump, the negative conversion tower performs regeneration work, and after the regeneration is finished and cleaned, the regenerated positive resin is transferred to the positive resin tank for temporary storage by using nitrogen and ultrapure water provided by a user. In order to further improve the regeneration effect, a heat exchanger is used for heating the regeneration liquid in the regeneration process. The negative resin tank is used for storing regenerated negative resin from the negative converter, and can be prepared by using common resin to obtain a polyethylene storage tank. Considering the mixing ratio of the mixed bed resin, the volume of the female resin tank needs to be larger than that of the male resin tank, and in some embodiments of the invention, the volume ratio of the male resin tank to the female resin tank is 1: 2-3. In some embodiments of the invention, the female half product tank and the female resin tank have the same volume.
The resin mixing and detecting assembly comprises a male measuring tank, a female measuring tank, a mixing tank and a resin detecting device, and one or more devices can be arranged in each device. The male metering groove and the female metering groove are used for accurately metering the male resin and the female resin from the male resin groove and the female resin groove respectively according to the mixing ratio, and in some specific embodiments of the invention, the male metering groove and the female metering groove are provided with scales and wheels at the bottoms for convenient movement and metering. One or more mixing tanks may be provided, and in some embodiments of the present invention, two mixing tanks are provided for mixing the regenerated male resin and the regenerated female resin in a mixing ratio. After the volume is measured in the metering tank, the resin is mixed in the mixing tank, and the accuracy of the proportion of the resin is high. The resin detection device is used for detecting the resin sampled from the mixing tank. In some embodiments of the present invention, the resin detection device checks the resistivity, the micro-particles, and/or the TOC, etc., of the mixed resin produced water. And filling the qualified resin into a resin turnover barrel for standby preservation.
Fig. 1 is a schematic plan view of a resin off-line recycling apparatus according to a first embodiment of the present invention. As shown in fig. 1, the resin off-line regeneration device of the present invention is designed in a skid-mounted manner, and is divided into 4 components according to factors such as function, simple piping and easy assembly and disassembly: the resin separation assembly, the positive resin regeneration assembly, the negative resin regeneration assembly, the resin mixing and detecting assembly, 4 assemblies are arranged in sequence along a first direction and occupy a rectangular area of a predetermined area. The resin separation component comprises a resin feeding device 11 and a separation tower 12, and has the main function of separating mixed anion and cation resins; the positive resin regeneration component: comprises a positive semi-finished product tank 13, a positive conversion tower 15 and a positive resin tank 17, and has the main function of adding medicine into the separated positive resin for regeneration and recovering the use function of the resin; the negative resin regeneration component: comprises a female semi-finished product tank 14, a female conversion tower 16, a female resin tank 18 and a heat exchanger 23, and mainly has the functions of adding medicine into the separated female resin for regeneration and recovering the use function of the female resin; resin mixing and detection assembly: comprises a positive measuring tank 19, a negative measuring tank 20, a mixing tank 21 and a resin detection device 22, and has the main functions of mixing the regenerated resins according to the proportion and detecting the mixed resins (mainly testing the water outlet effect). The four modules are arranged in sequence along a first direction shown in fig. 1 to occupy a rectangular area of a predetermined area as a whole
Fig. 2 is a schematic view of the piping arrangement of the resin off-line regeneration apparatus according to the first embodiment of the present invention. The resin off-line regeneration device comprises: a resin feeding device 11 for transferring the failure resin from the resin feeding device 11 to a separation tower 12, separating the cation resin and the anion resin in the separation tower 12, and switching through a valve, wherein the cation resin at the lower layer enters a cation semi-product groove 13 for temporary storage, and the anion resin at the upper layer enters a anion semi-product groove 14 for temporary storage; after the positive resin in the positive semi-finished product groove 13 is cleaned, the positive resin is transferred to a positive conversion tower 15 for standby by using a pneumatic diaphragm pump, and after the negative resin in the negative semi-finished product groove 14 is cleaned, the negative resin is transferred to a negative conversion tower 16 for standby by using the pneumatic diaphragm pump; switching the resin in the anode conversion tower 15 through a valve, adjusting the hydrochloric acid solution by using a medicine and ultrapure water provided by a user, carrying out regeneration work by going up and down, and after the regeneration is finished and the resin is cleaned, transferring the regenerated anode resin to an anode resin tank 17 by using the nitrogen and the ultrapure water provided by the user for temporary storage; the resin in the negative conversion tower 16 is switched by a valve, the resin is adjusted into a sodium hydroxide solution by using a medicine and ultrapure water provided by a user, the sodium hydroxide solution enters from the top to the bottom for regeneration, the heat exchanger 23 is used for heating the regenerated liquid at the same time, the regeneration effect is improved, and after the regeneration is finished and the resin is cleaned, the regenerated negative resin is transferred to the negative resin tank 18 by using the nitrogen and the ultrapure water provided by the user for temporary storage; in order to ensure the accurate mixing ratio, the positive resin in the positive resin tank 17 is transferred to the positive metering tank 19 by using a pneumatic diaphragm pump for accurate metering, and the negative resin in the negative resin tank 18 is transferred to the negative metering tank 20 by using the pneumatic diaphragm pump for accurate metering; after the respective metering of the cation and anion resins is completed, the resins are put into a mixing tank 21 for standby by using a pneumatic diaphragm pump according to the sequence of anion and cation; after the anion and cation resins in the mixing tank 21 are cleaned, firstly, nitrogen used by a user is used for mixing, and then, a pneumatic diaphragm pump is used for pumping and circulating through a pipeline mixer in the mixing tank 21 for mixing again, so that the resins are fully mixed; after the resin in the mixing tank 21 is mixed, the resin is sampled into a resin detection device 22, TOC, resistivity and/or microparticles of inlet and outlet water are measured, the regeneration effect of the resin is ensured to meet the use requirement of a customer, and then the mixed resin is transferred to a turnover box for storage through valve switching.
The resin off-line regeneration device disclosed by the invention preferably only comprises the equipment, the existing equipment of users is used for water supply, acid and alkali medicines and the like, the waste water is discharged to the existing neutralization equipment of users, and dosing equipment and neutralization equipment do not need to be additionally arranged, so that the production cost can be reduced.
< method for in situ regeneration of ion exchange resin offline >
The invention provides a method for carrying out off-line regeneration on ion exchange resin on site, which comprises the step of carrying out on-site regeneration on the resin user of the movable combined type resin off-line regeneration device so as to regenerate the resin which is out of service for the resin user.
The method has no time for transporting the resin to a resin factory, can reduce the risk of resin pollution, can directly recover the operation of the regenerated resin at a user site, has no risk of TOC dissolution, and needs short flushing time, while the resin generally transported to the resin factory for regeneration has the possibility of TOC dissolution because the resin is transported after regeneration, and generally needs to spend longer time for flushing in order to reduce the TOC. The overall resin regeneration and delivery cycle is significantly shortened.
In order to improve the resin regeneration effect and reduce the cost, the method comprises the step of regenerating the resin by using ultrapure water of a resin user. In some preferred embodiments of the present invention, the ultrapure water of the resin user is prepared by an ultrapure water system, the water quality is guaranteed, and the fine particles and trace metals are stable, whereas the pure water adopted in a general resin factory is unstable, and has an adverse effect on the resin regeneration effect. In some embodiments of the invention, the resin user provides ultrapure water having a resistivity of >18M Ω. cm and TOC <30ppb, corresponding to mixed bed produced water. The regeneration water meeting the above requirements is advantageous for controlling the quality of resin regeneration. In addition, the invention is matched with various detections in the resin regeneration process to ensure the quality.
In some embodiments of the present invention, the method for off-line regeneration of an ion exchange resin comprises:
i. resin input step:
and taking out the failed resin to be regenerated by the user from the user existing device, and placing the resin in the resin feeding device. The resin put into the resin input device is transferred to the separation tower through the pneumatic diaphragm pump, and the outlet of the pneumatic diaphragm pump is connected with the input pipeline to transfer the resin to the top of the separation tower.
A resin separation step:
and backwashing the failed resins in the separation tower by using nitrogen and filtered water provided by a user to separate the anion and cation resins. In some embodiments of the invention, the step of performing comprises: opening an exhaust valve of the separation tower and a water inlet valve at the top to fill the separation tower with water; opening a top water inlet valve and a bottom water discharge valve, and carrying out resin forward washing for 15-30 min by enabling washing water to enter upwards and leave downwards; opening a top exhaust valve and a bottom drain valve to drain water locally, and draining the separation tower to a liquid level of 3-5 m; opening an exhaust valve and a nitrogen inlet valve at the top of the separation tower, and aerating the resin in the separation tower for 50-70 min; and opening a water inlet valve at the bottom, and backwashing the backwashing drainage valve by using resin for 40-70 min.
The water used in the step is filtered water provided by a user, and in some embodiments of the invention, the filtered water has conductivity of 100-1000 us/cm, SDI <3, turbidity <1NTU, and residual chlorine <0.1ppm, and in some embodiments of the invention, the filtered water is produced by an activated carbon filter. The purity of the user-supplied nitrogen used in the present invention reaches 99.99%.
A pre-regeneration detection step:
after the separation is finished, the valve is switched, the lower layer of the male resin enters the male semi-finished product groove for temporary storage, and the upper layer of the female resin enters the female semi-finished product groove for temporary storage. In order to better control the resin regeneration effect, in some embodiments of the invention, the degree of contamination of the positive resin and the negative resin is evaluated separately at the outlet of the separation column.
In some embodiments of the present invention, the mixing rate of the male resin and the female resin is measured before the male half product tank and the female half product tank are transferred. Sampling valves are provided in the pipes transferred to the male half product tank and the female half product tank, and the mixing rate is detected by the sampling valves. The mixing rate test can evaluate the mixing rate of the cation resin in the anion resin or the mixing rate of the anion in the cation resin. If the mixing rate is not detected to a predetermined value, the mixture is fed to the separation tower again for separation, and if the mixing rate is detected to be qualified, the mixture is transferred to the male half product tank and the female half product tank. In some preferred embodiments of the present invention, the mixing ratio is controlled to not more than 0.5%, which is a volume percentage.
A cation resin regeneration step:
after the cation resin in the cation semi-finished product tank is cleaned, the cation resin is transferred to a cation conversion tower by using a pneumatic diaphragm pump, and the cation resin is regenerated in the cation conversion tower by using a medicine and ultrapure water provided by a resin user. In some embodiments of the invention, the step of performing comprises: after cleaning the cation resin in the cation semi-finished product tank, transferring the cation resin to the top of the cation conversion tower by using a pneumatic diaphragm pump, and opening a water inlet valve at the bottom and a backwashing water discharge valve to carry out resin backwashing for 20-40 min; opening a top water inlet valve and a bottom water discharge valve, and carrying out resin forward washing for 15-30 min; opening a medicine feeding valve and a medicine diluting water valve, starting a medicine feeding pump, feeding medicine for 50-70 min, and adjusting the flow rate to enable the concentration of the mixed medicine and diluting water to reach 3% -8%, and preferably 5% hydrochloric acid solution, wherein the medicine diluting water is selected from ultrapure water provided by a user; opening a middle water inlet valve and a bottom water discharge valve to clean the medicines; the resin discharge valve and the nitrogen gas inlet valve were opened, and the regenerated cation resin was transferred to the cation resin tank by using nitrogen gas and ultrapure water.
The drug dilution water referred to in this step is from user-supplied ultrapure water, which in some embodiments of the invention has a resistivity of >18M Ω -cm and TOC <30 ppb. The medicine used in the step is HCl medicine provided by a user, and the concentration of the HCl medicine is 10-30%.
A negative resin regeneration step:
and (3) after cleaning the cathode resin in the cathode semi-product groove, transferring the cleaned cathode resin to a cathode conversion tower by using a pneumatic diaphragm pump, and regenerating the cathode resin in the cathode conversion tower by using a medicine and ultrapure water provided by a resin user. In some embodiments of the invention, the step of performing comprises: transferring the resin in the negative resin semi-finished product tank to the top of a negative conversion tower through a pneumatic diaphragm pump, opening a water inlet valve at the bottom, and carrying out resin backwashing for 20-40 min by using a backwashing water discharge valve; opening a top water inlet valve and a bottom water discharge valve, and carrying out resin forward washing for 15-30 min; before medicine feeding, the diluting water required by medicine feeding is heated to 30-50 ℃ through a heat exchanger so as to further improve the regeneration effect; opening a medicine feeding valve and a medicine dilution water valve, starting a medicine feeding pump at the moment, feeding medicines for 100-150 min, and adjusting the flow to enable the concentration of the mixed medicine and dilution water to reach 1-5%, and further preferably 1-3% of sodium hydroxide solution; opening a middle water inlet valve and a bottom water discharge valve to clean the medicines; the resin discharge valve and the nitrogen gas inlet valve were opened, and the regenerated negative resin was transferred to the negative resin tank by using nitrogen gas and ultrapure water.
The drug dilution water referred to in this step is from user-supplied ultrapure water, which in some embodiments of the invention has a resistivity of >18M Ω -cm and TOC <30 ppb. The medicine used in the step is NaOH medicine provided by a user, and the concentration of the NaOH medicine is 10-30%.
v. resin mixing and detection step
In order to ensure accurate mixing ratio, the resin needs to be accurately metered by a positive metering tank and a negative metering tank before being mixed. In some embodiments of the invention, the mixing volume ratio of the male resin to the female resin is 1: 2-3, and the mixing ratio is further set to be 1:3 according to the actual mixing requirement of a user.
In some embodiments of the invention, the step of performing comprises: the positive resin in the positive resin tank is transferred to a positive metering tank for accurate metering by using a pneumatic diaphragm pump according to a preset amount, and the negative resin in the negative resin tank is transferred to a negative metering tank for accurate metering by using the pneumatic diaphragm pump according to the preset amount; and after the positive and negative resins are respectively metered, putting the positive and negative resins into a mixing tank for later use by using a pneumatic diaphragm pump according to the sequence of first negative and then positive. Opening a water inlet valve at the top, and replenishing water in the mixing tank to be 20-50 mm above the resin surface; opening a nitrogen gas inlet valve, and introducing nitrogen gas into the mixing tank for mixing; opening a drain valve at the bottom, and draining the liquid level of the mixing tank until the liquid level is equal to the resin surface; open bottom discharge valve, pneumatic pump export backward flow valve, use the circulation of pneumatic diaphragm pump to mix once more through PVC pipeline mixer to further ensure that the resin mixes fully.
After the resin in the mixing tank is mixed, the mixed resin is sampled into a resin detection device, TOC, micro-particles, resistivity and the like of inlet and outlet water are measured, the regeneration effect of the resin is ensured to meet the use requirement of a user, and then the mixed resin is transferred to a turnover box for storage through a pneumatic diaphragm pump by switching of a valve. In some embodiments of the invention, other than for accessBesides the detection of TOC, micro-particles and resistivity of water, the method also analyzes Na, K, CU, Fe, Zn and Cl ions in water and SiO2The concentration is analyzed and is controlled within a qualified range.
The method of the invention is adopted to carry out the off-line regeneration of the ion exchange resin, fully utilizes the ultrapure water of users as a regeneration water source, and is beneficial to further improving the regeneration effect; by adjusting and optimizing the regeneration specific steps, the whole regeneration period is short, the regeneration efficiency is high, in some specific embodiments of the invention, under the condition of regenerating the same amount of resin (such as 5000L), the transportation-free regeneration device has no transportation time, the time required by regeneration and the flushing time required by recovery operation are short, the regeneration and delivery periods can be greatly shortened, and the whole delivery period can be shortened by more than 5 days compared with the whole delivery period of regeneration of a common resin factory. The method of the invention combines a plurality of on-line detections, can better control the regeneration effect of the resin, because the regeneration is carried out in situ, the mixing can be carried out and the effluent quality can be measured after the resin regeneration is finished, and the effluent quality can not be detected in advance because a common resin factory does not involve mixing. The utilization of the equipment such as the yin-yang semi-finished product tank, the yin-yang metering tank and the like in the device ensures that the mixing ratio accuracy of the resin is high, and the independent pneumatic diaphragm pumps are used for transferring the resin in each step and are not mixed, so that the cross contamination of the resin is further prevented.
The method of the invention can be suitable for the regeneration of ion exchange resins with different specifications. In combination with the use scenario of the present invention, the method of the present invention is particularly suitable for regenerating mixed bed resins (such as model 650, 550, M800, S200, and the like, specifically including DOW model Ambertec UP650H, Ambertec UP550OH, LANXESS model Lewatit MonoPlus M800KR (OH), Lewatit MonoPlus S200KR (H), and the like) of ultrapure water systems. The mixed bed resin of the ultrapure water system means a ready-to-use resin which is composed of cation exchange resin and anion exchange resin and has been regenerated and premixed. The method of the invention is suitable for the electronic industry, in particular to the semiconductor and liquid crystal industry, such as the production fields of monocrystalline silicon, semiconductor wafer cutting and manufacturing, semiconductor chips, semiconductor packaging, lead frame, integrated circuits, liquid crystal displays, conductive glass, kinescopes, circuit boards, optical communication, computer components, capacitor cleaning products, various components and the like.
The present invention will be described in more detail with reference to examples and comparative examples, but the present invention is not limited to the examples.
Examples
Example 1
This example uses a mobile combined off-line resin regeneration apparatus as shown in fig. 1 and 2, which has 4 modules. The movable combined type resin off-line regeneration device is installed on the site of a certain liquid crystal enterprise, and is used for regenerating mixed bed resin (also called polishing resin) of an ultrapure water system which is stored for 2 years for the user.
Nitrogen provided by a user and the purity is 99.99 percent; the conductivity of the filtered water provided by a user is 100-1000 us/cm, the SDI is less than 3, the turbidity is less than 1NTU, and the residual chlorine is less than 0.1 ppm; ultrapure water provided by a user, the resistivity is more than 18M omega cm, and the TOC is less than 30 ppb; the concentration of HCl drug provided by a user is 10% -30%, and the HCl drug is analytically pure; the concentration of NaOH medicine provided by the user is 10% -30%, and the analysis is pure.
5000L of the mixed bed resin was charged into a resin charging device. Transferring the resin into a separation tower by using a pneumatic diaphragm pump, wherein an outlet of the pneumatic diaphragm pump is connected with an inlet pipeline to transfer the resin to the top of the separation tower; opening an exhaust valve of the separation tower and a water inlet valve at the top to fill the separation tower with water; opening a top water inlet valve and a bottom water discharge valve, and carrying out resin forward washing for 20min by using washing water which enters from top to bottom; opening a top exhaust valve and a bottom drain valve to drain water locally, and draining the separation tower to a liquid level of 4 m; opening an exhaust valve and a nitrogen inlet valve at the top of the separation tower, and aerating the resin in the separation tower for 60 min; opening a water inlet valve at the bottom, and carrying out resin backwashing on a backwashing drainage valve, wherein the flow speed of flushing water is 10m/h and is 60 min; under the backwashing state (the flow rate is 10m/h), opening a negative resin taking-out valve, and taking out the negative resin to a negative resin semi-product tank; in the backwashing state (flow rate 20m/h), the negative resin take-out valve was opened, and the positive resin was taken out to the positive resin semi-finished product tank. The sampling valves were provided in the pipes transferred to the male half product tank and the female half product tank, and the results of the mixing rate detection were shown in table 1. The mixing ratio is obtained by counting the number of the anion and cation resins.
Transferring the resin in the cation resin semi-finished product tank to the top of the cation conversion tower through a pneumatic diaphragm pump, opening a water inlet valve at the bottom, and carrying out resin backwashing for 30min by a backwashing water discharge valve; opening a top water inlet valve and a bottom water discharge valve, and carrying out resin forward washing for 20 min; opening a medicine inlet valve (HCl medicine provided by a user) and a medicine dilution water valve, starting a medicine adding pump at the moment, adjusting the flow of the medicine to enable the concentration of hydrochloric acid after the medicine and the dilution water are mixed to reach 5%, and feeding for 60 min; opening a middle water inlet valve and a bottom water discharge valve to clean the medicines; the resin discharge valve and the nitrogen gas inlet valve are opened, and the regenerated cation resin is transferred to the cation resin tank by using nitrogen gas and ultrapure water supplied by a user.
Transferring the resin in the negative resin semi-finished product tank to the top of a negative conversion tower through a pneumatic pump, opening a water inlet valve at the bottom, and carrying out resin backwashing for 30min by using a backwashing water discharge valve; opening a top water inlet valve and a bottom water discharge valve, and carrying out resin forward washing for 20 min; before medicine feeding, heating the dilution water required by medicine feeding to 35 ℃ by a heat exchanger; opening a medicine inlet valve (sodium hydroxide medicine provided by a user) and a medicine dilution water valve, starting a medicine adding pump at the moment, and adjusting flow medicine to enable the concentration of the sodium hydroxide mixed by the medicine and the dilution water to reach 2%; opening a middle water inlet valve and a bottom water discharge valve to clean the medicines; the resin discharge valve and the nitrogen gas inlet valve were opened, and the regenerated negative resin was transferred to the negative resin tank by using nitrogen gas and ultrapure water supplied from the user.
Transferring the resin in the cation resin storage tank into a metering tank by a pneumatic pump according to a preset amount; transferring the resin in the anion resin storage tank into a metering tank by a pneumatic pump according to a preset amount; transferring the metered anion-cation resin and cation resin into a mixing tank through a pneumatic diaphragm pump; opening a water inlet valve at the top, and supplementing water to the resin surface by 30mm through a mixing tank; opening a nitrogen gas inlet valve, and introducing nitrogen gas into the mixing tank for mixing; opening a drain valve at the bottom, and draining the liquid level of the mixing tank until the liquid level is equal to the resin surface; the bottom discharge valve, the pneumatic pump outlet reflux valve were opened and the mixing was again performed using the pneumatic diaphragm pump circulation through the mixer. After the resin in the mixing tank is mixed, sampling is carried out to a resin detection device, and then the resin is detectedDetermining resin breakage rate and total exchange capacity (i.e. the mole number of ion exchange groups contained in unit volume of ion exchange resin), and measuring TOC, microparticle, resistivity and SiO of inlet and outlet water by using online instrument2And referring to the results in tables 1 and 2, the inlet water is the outlet water of the ultraviolet oxidation device on the user site, the regeneration effect of the resin is ensured to meet the use requirement of the user, and then the mixed resin is transferred to a turnover box for storage through the valve switching and the pneumatic diaphragm pump.
Table 1 example 1 resin regeneration effect data
Table 2 example 1 water quality monitoring of mixed resins
| Analysis item | Unit of | Water inflow value | Water output value |
| Resistivity of | MΩ·cm | 14.5 | 18.24 |
| Micro-particles | Pcs/ml,>0.2um | -- | 2.4 |
| TOC | μg/L | 6 | 5 |
| SiO2 | μg/L | 1.0 | 1.0 |
As can be seen from Table 1, the analysis items of the invention are more than other resin regeneration enterprises, the regeneration quality of the resin can be better controlled through a plurality of detections, and the method of the invention has high accuracy of the resin mixing ratio and good resin regeneration effect. As can be seen from Table 2, the quality of the effluent of the regenerated mixed resin can meet the requirement of ultrapure water, and the regeneration effect of the resin can meet the use requirement of a user.
The above examples are intended only to illustrate several embodiments of the present invention, which are described in more detail and detail, but are not to be construed as imposing any limitation on the scope of the present invention. It should be clear that a person skilled in the art can make several variations and modifications without departing from the inventive concept, which fall within the scope of protection of the present invention.
Claims (10)
1. A method for off-line regeneration of ion exchange resin on site is characterized in that a movable combined off-line resin regeneration device is arranged on a resin user site to regenerate the resin which is failed by the resin user;
the device mainly comprises: the resin separation assembly, the positive resin regeneration assembly, the negative resin regeneration assembly and the resin mixing and detecting assembly;
the method comprises the steps of backwashing and separating the failed resin in the resin separation assembly by using nitrogen and filtered water provided by the resin user; and regenerating the resin in the positive resin regeneration assembly and the negative resin regeneration assembly by adopting the medicine and the ultrapure water provided by the resin user.
2. The method according to claim 1, wherein the resin off-line regeneration apparatus further comprises a plurality of holders by which the resin separation module, the male resin regeneration module, the female resin regeneration module, and the resin mixture detection module are assembled together in a detachable manner from each other.
3. The method of claim 1 or 2, wherein the resin separation module comprises a resin input device and a separation column, and the resin mixing and detecting module comprises a male metering tank, a female metering tank, a mixing tank, and a resin detecting device.
4. The method of claim 1 or 2, wherein the male resin regeneration assembly comprises a male semi-product tank, a male converter tower and a male resin tank and the female resin regeneration assembly comprises a female semi-product tank, a female converter tower, a female resin tank and a heat exchanger.
5. The method according to claim 3 or 4, further comprising transferring the separated male resin and female resin to a male semi-product tank and a female semi-product tank for temporary storage respectively; and respectively detecting the mixing rate of the positive resin and the negative resin before transferring to the positive semi-finished product groove and the negative semi-finished product groove.
6. The method according to any one of claims 3 to 5, further comprising transferring the regenerated male resin and the regenerated female resin to a male resin tank and a female resin tank, respectively, using nitrogen and ultrapure water supplied from the resin user after the regeneration is completed, and transferring the male resin and the regenerated female resin to the male metering tank and the female metering tank, respectively, for precise metering before the resins enter the mixing tank.
7. The method of claim 6, further comprising metering, charging into a mixing tank in order of yin first and yang second, cleaning the resin of the yin and yang in the mixing tank, and mixing thoroughly.
8. The method according to any one of claims 1 to 7, further comprising sampling the mixed resin to a resin detection device to determine the total organic carbon content, resistivity, particulates, SiO of the effluent2Content and/or ion content analysis.
9. The method according to any one of claims 1 to 8, wherein the resin user provides ultrapure water having a resistivity of >18M Ω -cm and TOC <30 ppb.
10. The method of any one of claims 1 to 9, wherein the resin is a polishing mixed bed resin used in ultrapure water systems.
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| CN113731515A (en) * | 2021-09-24 | 2021-12-03 | 蚌埠市天星树脂有限责任公司 | Regeneration method of waste cation exchange resin |
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| CN113731515A (en) * | 2021-09-24 | 2021-12-03 | 蚌埠市天星树脂有限责任公司 | Regeneration method of waste cation exchange resin |
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