CN114618462A - Failure regeneration method of brine iodine removal adsorbent - Google Patents
Failure regeneration method of brine iodine removal adsorbent Download PDFInfo
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- CN114618462A CN114618462A CN202210310854.4A CN202210310854A CN114618462A CN 114618462 A CN114618462 A CN 114618462A CN 202210310854 A CN202210310854 A CN 202210310854A CN 114618462 A CN114618462 A CN 114618462A
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- brine
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
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- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
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- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a regeneration method for brine iodine removal adsorbent failure, relates to the technical field of brine refining, and solves the technical problems of direct scrapping and high cost after adsorbent failure. The method for regenerating the brine iodine removal adsorbent in failure comprises the following steps: step S1, judging whether the adsorbent is invalid or not, if so, adjusting the flow of brine; step S2, adding a first treating agent into the brine for pH value adjustment; step S3, the brine with the adjusted pH value enters an adsorption tower to regenerate the adsorption capacity; and S4, allowing the brine flowing out of the adsorption tower to enter a wastewater system for collection and treatment. The invention is used for the regeneration of the adsorbent in case of failure, and is a method for achieving the regeneration of the iodine removal adsorbent and recovering the adsorption capacity by changing the operation mode, thereby greatly saving the production cost and improving the production efficiency.
Description
Technical Field
The invention relates to the technical field of brine refining, in particular to a brine iodine removal adsorbent failure regeneration method.
Background
Iodine in the brine is mainly represented by I-The ion form exists, and the ionic membrane manufacturer requires that the iodine content in the secondary refined brine is less than 200 ug/L. Iodine enters the electrolytic bath along with the brine and is oxidized into IO in the anolyte3-，IO3-In alkaline stripsUnder the device will be oxidized to IO4-Depositing on the ionic membrane in an anionic form; when IO is3-When the mass fraction of (A) exceeds 1000ug/L, the compound is reacted with Na+Precipitate is formed, when the mass fraction is less than 1000ug/L, the precipitate will react with Ba2+、Ca2+、Mg2+Insoluble barium periodate, calcium periodate and magnesium periodate are generated in a combined way; IO in the film even if the contents of barium, calcium and magnesium are extremely low4-And may form deposits with them and have different degrees of influence on current efficiency and cell voltage. If the iodine in the brine exceeds the control index, the accumulation of iodine can be formed after long-term operation, the current efficiency is reduced, and the service life of the ionic membrane is shortened.
For improving the service life of the ionic membrane, the pair I is required-Treating the ions by first treating I-Ion treatment to form iodine simple substance (I)2) In the form of:
2I-+2e＝I2
I2+Cl-→I2Cl-
I2Cl-in the presence of Cl-The solution of ions is easy to be adsorbed on the composite adsorbent, so as to achieve the purpose of removing iodine.
The method comprises the following specific steps: as shown in figure 1, brine firstly enters a filter for filtration, then a treating agent 1 (hydrochloric acid) is added through a mixer to adjust the pH value, a treating agent 2 (oxidant) is added through a mixer to react in a reaction tank 1 and a reaction tank 2, and then the obtained product enters an adsorption tower for adsorption and iodine removal, and after the iodine content meets the index requirement, a treating agent 3 (caustic soda) is used for neutralization and partial alkalinity, and then the obtained product is sent to primary brine for primary brine refining.
The applicant has found that the prior art has at least the following technical problems:
in the existing brine iodine removal technology, after an adsorbent in an adsorption tower fails, the iodine removal device is suspended, the failed adsorbent is taken out and discarded, and then a new adsorbent is placed into the adsorption tower.
Disclosure of Invention
The invention aims to provide a regeneration method for the failure of an adsorbent for removing iodine from brine, which aims to solve the technical problems of direct scrapping and high cost of the adsorbent after failure in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a method for regenerating an iodine removal adsorbent for brine in a failure mode, which comprises the following steps:
step S1, judging whether the adsorbent is invalid or not, if so, adjusting the flow of brine;
step S2, adding a first treating agent into the brine for pH value adjustment;
step S3, the brine with the adjusted pH value enters an adsorption tower to regenerate the adsorption capacity;
and S4, allowing the brine flowing out of the adsorption tower to enter a wastewater system for collection and treatment.
As a further improvement of the present invention, the adjustment of the brine flow rate in step S1 is to reduce the brine flow rate.
As a further improvement of the invention, the flow rate of the brine is reduced to 20m3-30m3/h。
As a further improvement of the present invention, the first treating agent in step S2 is 31% hydrochloric acid.
As a further improvement of the invention, the pH value is adjusted to 1.5-2.5 in step S2.
As a further improvement of the invention, the method also comprises a step S5 of periodically sampling to detect the iodine content in the brine, and when the iodine content in the brine reaches a set target value, the flow rate of the brine is increased and the normal production treatment step is executed.
As a further improvement of the present invention, in step S5, the normal production processing step includes
Step A1, filtering the brine through a sand filter, adding the first treating agent and the second treating agent, and uniformly mixing;
step A2, the mixed brine enters an adsorption tower to be subjected to iodide ion adsorption treatment;
step A3, enabling the brine after iodine ion adsorption to flow out of the adsorption tower, and adding a third treating agent to adjust the pH value;
and step A4, feeding the adjusted brine into a brine refining process.
As a further improvement of the present invention, in step a1, the first treating agent is 31% hydrochloric acid, and the second treating agent is an oxidizing agent; in step a3, the third treating agent is 32% caustic soda solution.
As a further improvement of the present invention, in step A3, a third treating agent is added to adjust the pH to 7-9.
As a further improvement of the present invention, in step S5, the interval time of the periodic sampling is 8 hours; the set target value of the iodine content is an iodine content of less than 200 ppb.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a method for regenerating an iodine removal adsorbent for brine in a failure mode, which is a method for regenerating the iodine removal adsorbent and recovering the adsorption capacity by changing the operation mode, wherein on the basis of the original process, the operation mode is changed, an iodine removal system is quickly switched into the system, the influence of a large amount of iodine ions released by the adsorbent on a subsequent system is reduced, and the adsorption capacity is recovered by changing the operation mode and adding hydrochloric acid under the condition of small flow; through the treatment, the adsorption capacity of the ineffective adsorbent is recovered, so that the iodine removing device can normally operate, the production cost is greatly saved, and the production efficiency is improved.
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, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow diagram of a prior art process for removing iodine from brine;
FIG. 2 is a process flow diagram of the regeneration method for brine iodine removal adsorbent failure.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
As shown in fig. 2, the invention provides a method for regenerating a brine iodine removal adsorbent in a failure mode, which comprises the following steps:
step S1, judging whether the adsorbent is invalid or not, if so, adjusting the flow of brine;
step S2, adding a first treating agent into the brine for pH value adjustment;
step S3, the brine with the adjusted pH value enters an adsorption tower to regenerate the adsorption capacity;
and S4, allowing the brine flowing out of the adsorption tower to enter a wastewater system for collection and treatment.
The invention provides a method for regenerating an iodine removal adsorbent for brine in a failure mode, which is a method for regenerating the iodine removal adsorbent and recovering the adsorption capacity by changing the operation mode, wherein on the basis of the original process, the operation mode is changed, an iodine removal system is quickly switched into the system, the influence of a large amount of iodine ions released by the adsorbent on a subsequent system is reduced, and the adsorption capacity is recovered by changing the operation mode and adding hydrochloric acid under the condition of small flow; through the treatment, the adsorption capacity of the ineffective adsorbent is recovered, so that the iodine removing device can normally operate, the production cost is greatly saved, and the production efficiency is improved.
In step S1, the brine flow is adjusted to be decreased.
Specifically, the brine flow is reduced to 20m3-30m3/h。
Wherein, the first treating agent in step S2 is 31% hydrochloric acid.
In step S2, the PH is adjusted to 1.5-2.5. After the iodine removing adsorbent loses adsorption capacity when exposed to an alkaline environment, in order to recover the adsorption capacity, the pH value of the brine needs to be adjusted to 1.5-2.5, and the regeneration is carried out at a flow rate of 20m3/h-30m3/h to recover the adsorption capacity.
Specifically, after the adsorbent loses adsorption capacity, the brine flow is controlled to be 20m3-30m3And h, adding 31% hydrochloric acid to control the pH value of the brine to be 1.5-2.5, stopping adding the oxidant, changing the brine out of the adsorption tower into a wastewater removal system for collection, sampling every 8 hours in the period until the iodine content of the brine is less than 200ppb, increasing the treatment load, adding the oxidant, merging the brine into a primary brine refining system, and recovering the normal production.
And step S5, periodically sampling to detect the iodine content in the brine, and when the iodine content in the brine reaches a set target value, increasing the flow of the brine and executing the normal production treatment step.
Wherein, in step S5, the normal production processing step includes
Step A1, filtering the brine through a sand filter, adding the first treating agent and the second treating agent, and uniformly mixing;
step A2, the mixed brine enters an adsorption tower to be subjected to iodide ion adsorption treatment;
step A3, enabling the brine after iodine ion adsorption to flow out of the adsorption tower, and adding a third treating agent to adjust the pH value;
and step A4, feeding the adjusted brine into a brine refining process.
In the step A1, the first treating agent is 31% hydrochloric acid, and the second treating agent is an oxidizing agent; in step a3, the third treating agent is 32% caustic soda solution.
Wherein, in the step A3, a third treating agent is added to adjust the pH value to 7-9.
In step S5, the interval time of the periodic sampling is 8 hours; the set target value of the iodine content is an iodine content of less than 200 ppb.
The normal production process flow comprises the following steps: filtering brine from a brine collection process by using a sand filter, adding 31% hydrochloric acid to adjust the pH value to 1.5-2.5, adding an oxidant, uniformly mixing in a mixer, sequentially and respectively entering a reaction tank 1, a reaction tank 2 and a reaction tank 3, fully reacting, pumping into an adsorption tower by using a brine pump, adsorbing iodine ions in the brine under the adsorption action of a special adsorbent in the adsorption tower, finally adding 32% caustic soda solution, adjusting the pH value of the brine to 7-9, and then removing brine for refining. Through the adsorption of the adsorbent, the concentration of iodide ions in brine is effectively reduced, and the quality index of refined brine entering the electrolytic cell is qualified.
It should be noted that "inward" is a direction toward the center of the accommodating space, and "outward" is a direction away from the center of the accommodating space.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in fig. 1 to facilitate the description of the invention and to simplify the description, but are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered as limiting the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood according to specific situations by those of ordinary skill in the art.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. A regeneration method for brine iodine removal adsorbent failure is characterized by comprising the following steps:
step S1, judging whether the adsorbent is invalid or not, if so, adjusting the flow of brine;
step S2, adding a first treating agent into the brine for pH value adjustment;
step S3, the brine with the adjusted pH value enters an adsorption tower to regenerate the adsorption capacity;
and step S4, allowing the brine flowing out of the adsorption tower to enter a wastewater system for collection and treatment.
2. The brine iodine removing adsorbent regeneration method of claim 1 wherein the brine flow rate is adjusted to decrease the brine flow rate in step S1.
3. The brine de-iodination sorbent regeneration process of claim 2, wherein the reduced brine flow is reduced to 20m3-30m3/h。
4. The brine de-iodination adsorbent spent regenerating method of claim 1, wherein the first treating agent in step S2 is 31% hydrochloric acid.
5. The regeneration method of claim 1, wherein the pH value of the brine is adjusted to 1.5-2.5 in step S2.
6. The method of claim 1, further comprising a step S5 of periodically sampling to detect the iodine content in the brine, and increasing the brine flow rate and performing normal production treatment when the iodine content in the brine reaches a predetermined target value.
7. The regeneration method of claim 6, wherein the normal process step of S5 comprises
Step A1, filtering the brine through a sand filter, adding the first treating agent and the second treating agent, and uniformly mixing;
step A2, the mixed brine enters an adsorption tower to be subjected to iodide ion adsorption treatment;
step A3, enabling the brine after iodine ion adsorption to flow out of the adsorption tower, and adding a third treating agent to adjust the pH value;
and step A4, feeding the adjusted brine into a brine refining process.
8. The brine de-iodination sorbent regeneration process of claim 7, wherein in step a1, the first treatment agent is 31% hydrochloric acid and the second treatment agent is an oxidizing agent; in step a3, the third treating agent is 32% caustic soda solution.
9. The brine iodine removal adsorbent regeneration method of claim 7 wherein in step a3, a third treatment agent is added to adjust the PH to 7-9.
10. The brine iodine removal adsorbent regeneration method of claim 6, wherein in step S5, the periodic sampling interval is 8 hours; the set target value of the iodine content is an iodine content of less than 200 ppb.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210310854.4A CN114618462A (en) | 2022-03-28 | 2022-03-28 | Failure regeneration method of brine iodine removal adsorbent |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210310854.4A CN114618462A (en) | 2022-03-28 | 2022-03-28 | Failure regeneration method of brine iodine removal adsorbent |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103071457A (en) * | 2013-01-15 | 2013-05-01 | 中国科学院青海盐湖研究所 | Gel type iodine ion adsorbent and preparation method and application thereof |
| CN110194501A (en) * | 2019-04-30 | 2019-09-03 | 凯莱英医药化学（阜新）技术有限公司 | From the continuous process and continuous device for recycling iodide in waste water containing iodine |
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- 2022-03-28 CN CN202210310854.4A patent/CN114618462A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103071457A (en) * | 2013-01-15 | 2013-05-01 | 中国科学院青海盐湖研究所 | Gel type iodine ion adsorbent and preparation method and application thereof |
| CN110194501A (en) * | 2019-04-30 | 2019-09-03 | 凯莱英医药化学（阜新）技术有限公司 | From the continuous process and continuous device for recycling iodide in waste water containing iodine |
Non-Patent Citations (1)
| Title |
|---|
| 天津化工研究院等编: "《绿色精细化工--天然产品制造法（第4集）》", vol. 1, 科学技术文献出版社, pages: 350 - 352 * |
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