CN114904500B - Resin desorbing agent and desorption method - Google Patents
Resin desorbing agent and desorption method Download PDFInfo
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- CN114904500B CN114904500B CN202210145596.9A CN202210145596A CN114904500B CN 114904500 B CN114904500 B CN 114904500B CN 202210145596 A CN202210145596 A CN 202210145596A CN 114904500 B CN114904500 B CN 114904500B
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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
- 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
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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Abstract
The application discloses a resin desorbing agent and a desorption method, wherein the resin desorbing agent comprises an acid cleaning solution I, a saline-alkali and organic solvent cleaning solution II, wherein the acid cleaning solution I is hydrochloric acid 1.5-3BV with the weight percent of (2-8), the saline-alkali and organic solvent cleaning solution II is organic solvent solution 0.5-1BV with the weight percent of (2-5) NaOH+ (8-12) NaCl+ (20-30), the saline-alkali cleaning solution II is hydrochloric acid 0.5-1.5BV with the weight percent of (2-5) NaOH+ (8-12) NaCl solution 2-4BV, and the acid cleaning solution II is hydrochloric acid with the weight percent of (2-3). The technical scheme of this application has showing the desorption effect that has improved the contaminated resin.
Description
Technical Field
The invention belongs to the technical field of environmental protection, and particularly relates to a resin desorbing agent and a desorption method.
Background
In the industrial wastewater treatment process, organic matters are generally required to be adsorbed, so that the organic matters in the wastewater are removed, on one hand, the wastewater purification treatment is realized, and on the other hand, the blocking degree of the membrane in the subsequent membrane treatment can be reduced, and the service life of the membrane is prolonged.
In the prior art, resin is usually desorbed in situ in an adsorption tank after the resin in the adsorption tank reaches the working exchange capacity, the desorption mode is limited by the space and structural constraint of the adsorption tank, the desorption effect is not satisfactory, the commonly adopted desorption agents are acid and saline-alkali, the existing desorption agents and desorption process cannot meet the desorption requirement, organic matters still remain in the resin, the adsorption efficiency of the resin is seriously affected, and the wastewater purification cost is high.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a resin desorption agent and a desorption method.
A resin desorbing agent comprises an acid cleaning solution I, a saline-alkali and organic solvent cleaning solution, a saline-alkali cleaning solution and an acid cleaning solution II, wherein the acid cleaning solution I is (2-8) wt% hydrochloric acid 1.5-3BV, the saline-alkali and organic solvent cleaning solution I is (2-5) wt% NaOH+ (8-12) wt% NaCl+ (20-30) wt% organic solvent solution 0.5-1BV, the saline-alkali cleaning solution I is (2-5) wt% NaOH+ (8-12) wt% NaCl solution 2-4BV, and the acid cleaning solution II is (2-3) wt% hydrochloric acid 0.5-1.5BV.
Further, the mass percentage of the hydrochloric acid in the acid cleaning liquid II is smaller than that of the hydrochloric acid in the acid cleaning liquid I.
The desorption method adopting the resin desorbent comprises the following steps: transferring the resin in the adsorption tank to a desorption tank, and performing the following steps in sequence: acid cleaning, namely, saline-alkali and organic solvent cleaning, saline-alkali cleaning and acid cleaning.
Further, the acid cleaning one is: 1.5-3BV of (2-8) wt% hydrochloric acid is adopted, the temperature is 52-58 ℃, the washing is carried out in two steps, half of the dosage of each step is adopted, the first step is to be soaked for not less than 1 hour, compressed air is used for stirring in the soaking process, and then deionized water is used for washing.
Further, the cleaning of the saline-alkali and the organic solvent is as follows: (2-5) wt% NaOH+ (8-12) wt% NaCl+ (20-30) wt% organic solvent solution 0.5-1BV, at 52-58 deg.C, soaking for 2 hr, and washing with deionized water.
Further, the organic solvent is an organic acid, an organic alcohol, or a combination thereof.
Further, the organic acid is oxalic acid, acetic acid or citric acid; the organic alcohol is methanol or isopropanol.
Further, the saline-alkali cleaning is as follows: (2-5) NaOH+ (8-12) NaCl solution 2-4BV at 52-58 deg.C, cleaning in three steps, wherein the first step is soaking for at least 2 hr, washing with deionized water, and draining; in the second step, the soaking time is not less than 2 hours, compressed air is used for stirring in the soaking process, deionized water is used for washing after the soaking is finished, and the soaking is drained; two-thirds of the amount used in the third step was then rinsed with deionized water.
Further, the acid cleaning II comprises the following steps: (2-3) 0.5-1.5BV of hydrochloric acid with weight percent, normal temperature and finally washing with deionized water.
Further, the method also comprises the step of treating the elution waste liquid by adopting a wet oxidation process, wherein the wet oxidation process is as follows: adjusting the pH of the elution waste liquid to 2-4 by sulfuric acid, adding hydrogen peroxide according to the concentration of 2-5%, and uniformly mixing; heating the reaction tower to 145-150 ℃ by using steam, and then delivering the prepared stock solution into the reaction tower, wherein the effective residence time of the stock solution in the reaction tower is 1.5-2h.
Specifically, compared with the prior art, the invention has the advantages that: the technical scheme of this application is with the process that the resin jar in the prior art adsorbs and desorbs improve to "internal absorption + external desorption" process, has showing the desorption effect that has improved the contaminated resin. Specifically:
1. the desorption process outside the tank is more thorough, the operable degree is higher than that of the desorption in the adsorption tank, and the desorption efficiency is remarkably improved by adding compressed air for stirring.
2. The desorption liquid for desorbing the resin adsorbed with the organic matters is improved, the composition ratio of the desorption liquid is continuously tried to be adjusted, so that the desorption effect is optimal, the organic solvent is added in a breakthrough manner on the basis of the existing saline-alkali desorption liquid, unexpected excellent desorption effect is obtained, and the preferable content ratio of the organic solvent is determined through continuous try.
3. The desorption process is further optimized and improved, the consumption and the soaking time of each step in the desorption process are optimized, and the process parameter combination with excellent desorption effect is obtained.
4. The desorption waste liquid is treated by adopting a wet catalytic oxidation process, the removal rate of organic matters in the desorption waste liquid reaches more than 80 percent and can reach 92 percent at most, the high-efficiency removal of the organic matters can be realized, and the powerful guarantee is provided for the zero emission of industrial waste water.
Detailed Description
A resin desorbing agent comprises an acid cleaning solution I, a saline-alkali and organic solvent cleaning solution, a saline-alkali cleaning solution and an acid cleaning solution II, wherein the acid cleaning solution I is (2-8) wt% hydrochloric acid 1.5-3BV, the saline-alkali and organic solvent cleaning solution I is (2-5) wt% NaOH+ (8-12) wt% NaCl+ (20-30) wt% organic solvent solution 0.5-1BV, the saline-alkali cleaning solution I is (2-5) wt% NaOH+ (8-12) wt% NaCl solution 2-4BV, and the acid cleaning solution II is (2-3) wt% hydrochloric acid 0.5-1.5BV.
Preferably, the mass percent of hydrochloric acid in the acid cleaning solution II is smaller than the mass percent of hydrochloric acid in the acid cleaning solution I.
The desorption method adopting the resin desorbent comprises the following steps: transferring the resin in the adsorption tank to a desorption tank, and performing the following steps in sequence: acid cleaning, namely, saline-alkali and organic solvent cleaning, saline-alkali cleaning and acid cleaning.
Preferably, the resin in the adsorption tank is backwashed by air entrainment prior to transfer to fluff the resin.
Preferably, the acid wash one is: 1.5-3BV of (2-8) wt% hydrochloric acid is adopted, the temperature is 52-58 ℃, the washing is carried out in two steps, half of the dosage of each step is adopted, the first step is to be soaked for not less than 1 hour, compressed air is used for stirring in the soaking process, and then deionized water is used for washing.
The cleaning of the saline alkali and the organic solvent is as follows: (2-5) wt% NaOH+ (8-12) wt% NaCl+ (20-30) wt% organic solvent solution 0.5-1BV, at 52-58 deg.C, soaking for 2 hr, and washing with deionized water.
Preferably, the organic solvent is an organic acid, an organic alcohol, or a combination thereof.
Optionally, the organic acid is oxalic acid, acetic acid or citric acid; the organic alcohol is methanol or isopropanol.
The saline-alkali cleaning is as follows: (2-5) NaOH+ (8-12) NaCl solution 2-4BV at 52-58 deg.C, cleaning in three steps, wherein the first step is soaking for at least 2 hr, washing with deionized water, and draining; in the second step, the soaking time is not less than 2 hours, compressed air is used for stirring in the soaking process, deionized water is used for washing after the soaking is finished, and the soaking is drained; two-thirds of the amount used in the third step was then rinsed with deionized water.
Acid cleaning two is as follows: (2-3) 0.5-1.5BV of hydrochloric acid with weight percent, normal temperature and finally washing with deionized water.
Preferably, the method further comprises the step of treating the elution waste liquid by a wet oxidation process, wherein the wet oxidation process is as follows: adjusting the pH of the elution waste liquid to 2-4 by sulfuric acid, adding hydrogen peroxide according to the concentration of 2-5%, and uniformly mixing; heating the reaction tower to 145-150 ℃ by using steam, and then delivering the prepared stock solution into the reaction tower, wherein the effective residence time of the stock solution in the reaction tower is 1.5-2h.
After desorption, the resin was transferred back to the adsorption tank.
Specifically, desorption may be performed using the specific steps in table 1.
TABLE 1
With the extension of the operation time, the adsorption performance of the resin is generally reduced to below 80% of the initial adsorption performance after the conventional in-tank desorption mode is circulated for many times, the adsorption performance of the resin is difficult to be improved by in-tank desorption, the desorption degree of the resin can be obviously improved by adopting the desorption method in the application, the adsorption performance of the resin can be recovered to above 90% from below 80% of the original adsorption performance after the desorption is carried out by adopting the specific steps in table 1, and the desorption effect is obviously improved, so that the use cost of the resin can be greatly reduced.
Optionally, the elution waste liquid is treated by a wet oxidation process, wherein the wet oxidation process is as follows: adjusting the pH of the elution waste liquid to 2-4 by sulfuric acid, adding hydrogen peroxide according to the concentration of 2-5%, and uniformly mixing; heating the reaction tower to 145-150 ℃ by using steam, and then delivering the prepared stock solution into the reaction tower, wherein the effective residence time of the stock solution in the reaction tower is 1.5-2h.
The results of the elution waste liquid treated by the wet oxidation process are shown in Table 2. As shown in Table 2, the removal rate of the elution waste liquid is more than 80%, and the highest removal rate can reach 92%, so that the organic matters in the elution waste liquid can be efficiently removed, and the waste liquid can be discharged up to the standard.
TABLE 2
In the description of the present invention, it should be understood that the terms "center," "longitudinal," "transverse," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," etc. indicate orientations or positional relationships, merely for convenience in describing the present invention and to simplify the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be configured and operated in a particular orientation, and therefore should not be construed as limiting the present invention. Furthermore, features defining "first", "second" may include one or more such features, either explicitly or implicitly. In the description of the present invention, unless otherwise indicated, the meaning of "a plurality" is two or more.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
In the description of the present invention, a description of the terms "one embodiment," "some embodiments," "illustrative embodiments," "examples," "specific examples," or "some examples," etc., means 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 present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
While embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that: many changes, modifications, substitutions and variations may be made to the embodiments without departing from the spirit and principles of the invention, the scope of which is defined by the claims and their equivalents.
Claims (2)
1. A resin desorption method, which is characterized in that the method comprises the following steps: transferring the resin in the adsorption tank to a desorption tank, and sequentially performing the following steps: 1. backwashing, namely adopting DIW+compressed air, wherein the dosage is 1-3BV, the flow rate is 2-4BV/h, the water temperature is 50 ℃, the liquid is fed in a countercurrent manner, and the air is added for backwashing for the first 20 minutes; 2. draining the liquid from the gas cap, and draining backwash water in the tank; 3. acid cleaning: adopting (2-8) wt% hydrochloric acid of 1.5BV, flow rate of 1.5BV/h, water temperature of 54 ℃, countercurrent liquid inlet, circulating soaking for not less than 1 hour, air inlet stirring for 2-3 times, each time for 5 minutes; 4. acid cleaning: 1.5BV of (2-8) wt% hydrochloric acid, 1.5BV/h of flow rate and 54 ℃ of water temperature are adopted, and liquid is fed in countercurrent; 5. draining the liquid from the top of the gas, and draining the acid liquid in the tank; 6. washing: DIW is adopted, the dosage is 4BV, the flow speed is 3BV/h, the water temperature is 53 ℃, and the liquid is fed in countercurrent; 7. draining liquid from the gas cap, and draining liquid in the tank; 8. cleaning the saline-alkali and organic cleaning solution: (2-5) NaOH+ (8-12) NaCl+ (20-30) organic cleaning solution 0.5-1BV, 3BV/h flow rate, 56 ℃ water temperature, countercurrent liquid feeding, circulating soaking for not less than 2 hours, air inlet stirring for 3-4 times, each time for 5 minutes; the organic cleaning liquid is organic acid, organic alcohol or a combination thereof, and the organic acid is oxalic acid, acetic acid or citric acid; the organic alcohol is methanol or isopropanol; 9. draining liquid from the gas cap, and draining liquid in the tank; 10. washing with DIW, using 1BV, flowing at 3BV/h, water temperature of 56 ℃, and countercurrent feeding; 11. draining liquid from the gas cap, and draining liquid in the tank; 12. and (3) cleaning the salt and alkali: (2-5) NaOH+ (8-12) NaCl solution with weight percent of 0.5-1BV, 3BV/h flow rate, 56 ℃ water temperature, countercurrent liquid inlet, cyclic soaking for not less than 2 hours, air inlet and stirring for 3-4 times, each time for 5 minutes; 13. washing with DIW, using 1BV, flowing at 3BV/h, water temperature of 56 ℃, countercurrent liquid feeding, 14, gas top liquid discharging, and draining the liquid in the tank; 15. washing the salt and alkali, (2-5) NaOH+ (8-12) NaCl solution with the weight percent of 1-2BV, the flow rate of 1BV/h, the water temperature of 56 ℃, and countercurrent liquid inlet; 16. washing with DIW, using 1BV, flowing at 3BV/h, water temperature of 56 ℃, and countercurrent feeding; 17. washing with DIW, wherein the dosage is 1BV, the flow speed is 3BV/h, and the liquid is fed in countercurrent at normal temperature; 18. draining liquid from the gas cap, and draining liquid in the tank; 19. acid cleaning II: (2-3) hydrochloric acid 1BV with the flow rate of 0.5BV/h and normal temperature, and countercurrent liquid inlet; 20. draining liquid from the gas cap, and draining liquid in the tank; 21. washing with DIW, wherein the dosage is 1BV, the flow speed is 3BV/h, and the countercurrent liquid inlet is carried out; 22. and (3) forward washing, namely, adopting raw water with the flow rate of 6BV/h, and forward flowing liquid, flushing for 10 minutes, and recovering the adsorption performance of the resin from 80% of the original adsorption performance to more than 90% after desorption.
2. The method of claim 1, further comprising treating the elution waste liquid with a wet oxidation process comprising: adjusting the pH of the elution waste liquid to 2-4 by sulfuric acid, adding hydrogen peroxide according to the concentration of 2-5%, and uniformly mixing; heating the reaction tower to 145-150 ℃ by using steam, and then delivering the prepared stock solution into the reaction tower, wherein the effective residence time of the stock solution in the reaction tower is 1.5-2h.
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| JPS5673547A (en) * | 1979-11-16 | 1981-06-18 | Asahi Glass Co Ltd | Regeneration of anion exchange membrane |
| JP2001293380A (en) * | 2000-04-13 | 2001-10-23 | Ito En Ltd | Method for preparing ion-exchange resin and regeneration method |
| CN110237832B (en) * | 2019-05-29 | 2021-12-21 | 江苏南大环保科技有限公司 | Regeneration method of coking tail water adsorption resin |
| CN110316911A (en) * | 2019-07-24 | 2019-10-11 | 杭州深瑞水务有限公司 | A kind for the treatment of process of the high full qualified discharge of hardly degraded organic substance waste water |
| CN110711606A (en) * | 2019-10-24 | 2020-01-21 | 北京纬纶华业环保科技股份有限公司 | Method and system for treating waste ion exchange resin |
| CN112495453A (en) * | 2020-12-20 | 2021-03-16 | 衢州巨化锦纶有限责任公司 | Regeneration method of ion exchange resin for refining caprolactam |
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