CN114904500A - Resin desorption agent and desorption method - Google Patents

Resin desorption agent and desorption method Download PDF

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CN114904500A
CN114904500A CN202210145596.9A CN202210145596A CN114904500A CN 114904500 A CN114904500 A CN 114904500A CN 202210145596 A CN202210145596 A CN 202210145596A CN 114904500 A CN114904500 A CN 114904500A
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acid
saline
solution
cleaning solution
cleaning
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CN114904500B (en
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倪健
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Beijing Ome Environment Engineering Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/34Regenerating or reactivating
    • B01J20/345Regenerating or reactivating using a particular desorbing compound or mixture
    • B01J20/3475Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00Specific treatment goals
    • C02F2303/16Regeneration of sorbents, filters
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/62Plastics recycling; Rubber recycling

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Detergent Compositions (AREA)

Abstract

The application discloses a resin desorbent and a desorption method, wherein the resin desorbent comprises a first acid cleaning solution, a first saline-alkali + organic solvent cleaning solution, a second saline-alkali cleaning solution and a second acid cleaning solution, wherein the first acid cleaning solution is (2-8) wt% hydrochloric acid 1.5-3BV, the first saline-alkali + organic solvent cleaning solution is (2-5) wt% NaOH + (8-12) wt% NaCl + (20-30) wt% organic solvent solution 0.5-1BV, the second saline-alkali cleaning solution is (2-5) wt% NaOH + (8-12) wt% NaCl solution 2-4BV, and the second acid cleaning solution is (2-3) wt% hydrochloric acid 0.5-1.5 BV. The technical scheme of this application has shown the desorption effect that has improved contaminated resin.

Description

Resin desorption agent and desorption method
Technical Field
The invention belongs to the technical field of environmental protection, and particularly relates to a resin desorption agent and a desorption method.
Background
In the industrial wastewater treatment process, the adsorption of organic matters is usually needed, the organic matters in the wastewater are removed, on one hand, the purification treatment of the wastewater is realized, on the other hand, the blocking degree of the membrane during the subsequent membrane treatment can be reduced, and the service life of the membrane is prolonged.
Among the prior art, carry out the resin desorption in situ in the adsorption tank after the resin in the adsorption tank reaches work exchange capacity usually, this kind of desorption mode is subject to the space and the structural constraint of adsorption tank, and the desorption effect is not fully satisfactory, and the desorbent that adopts usually is sour and saline and alkaline moreover, and desorption demand can not be satisfied to current desorbent and desorption technology, causes the organic matter still to remain in the resin, seriously influences the adsorption efficiency of resin, causes waste water purification cost to remain high.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a resin desorbent and a desorption method.
A resin desorbent comprises an acid cleaning solution I, a saline-alkali + organic solvent cleaning solution, a saline-alkali cleaning solution and an acid cleaning solution II, wherein the acid cleaning solution I is 1.5-3BV of (2-8) wt% hydrochloric acid, the saline-alkali + organic solvent cleaning solution is 0.5-1BV of (2-5) wt% NaOH + (8-12) wt% NaCl + (20-30) wt% organic solvent solution, the saline-alkali cleaning solution is 2-4BV of (2-5) wt% NaOH + (8-12) wt% NaCl solution, and the acid cleaning solution II is 0.5-1.5BV of (2-3) wt% hydrochloric acid.
Further, the mass percent of the hydrochloric acid in the acid cleaning solution II is less than that of the hydrochloric acid in the acid cleaning solution I.
The desorption method adopting the resin desorption agent comprises the following steps: transferring the resin in the adsorption tank into a desorption tank, and carrying out the following steps in sequence: acid cleaning is carried out firstly, saline alkali + organic solvent cleaning is carried out, saline alkali cleaning is carried out, and acid cleaning is carried out secondly.
Further, the first acid cleaning step is as follows: adopting (2-8) wt% hydrochloric acid 1.5-3BV, temperature 52-58 deg.C, cleaning in two steps, half amount of each step, soaking in the first step for not less than 1 hr, stirring with compressed air, and washing with deionized water.
Further, the saline-alkali + organic solvent cleaning comprises the following steps: (2-5) NaOH (8-12) NaCl (20-30) and organic solvent solution 0.5-1BV at 52-58 deg.C for 2 hr, and then 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, saline-alkali cleaning comprises the following steps: (2-5) 2-4BV of NaOH + (8-12) wt% NaCl solution at 52-58 ℃, cleaning in three steps, wherein the soaking time in the first step is not less than 2 hours, then washing with deionized water and draining; in the second step, the soaking time is not less than 2 hours, the stirring is carried out by compressed air in the soaking process, and after the soaking is finished, the washing is carried out by deionized water and the water is drained; and thirdly, using two thirds of the dosage, and then washing with deionized water.
Further, acid cleaning is as follows: (2-3) 0.5-1.5BV of hydrochloric acid, 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 comprises the following steps: adjusting pH of the elution waste liquid to 2-4 with sulfuric acid, adding hydrogen peroxide according to the concentration of 2-5%, and mixing uniformly; heating the reaction tower to 145-150 ℃ by using steam, and then sending the prepared stock solution into the reaction tower, wherein the effective retention time of the stock solution in the reaction tower is 1.5-2 h.
Specifically, compared with the prior art, the invention has the advantages that: according to the technical scheme, the process of adsorption and desorption in the resin tank in the prior art is improved into the process of 'in-vivo adsorption + in-vitro desorption', and the desorption effect of the polluted resin is obviously improved. Specifically, the method comprises the following steps:
1. the desorption process is more thorough outside the jar, and the desorption is higher in the adsorption tank is compared to the operatable degree, through increasing the compressed air stirring, is showing and is improving desorption efficiency.
2. The desorption solution for desorbing the resin adsorbing the organic matters is improved, the composition ratio of the desorption solution is continuously tried to be adjusted, the desorption effect is optimal, the organic solvent is increased in a breakthrough manner on the basis of the existing saline-alkali desorption solution, the unexpected excellent desorption effect is obtained, and the optimal content ratio of the organic solvent is continuously tried to be determined.
3. The desorption process is further optimized and improved, the dosage 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 over 80 percent and can reach 92 percent at most, the organic matters can be efficiently removed, and the method provides powerful guarantee for zero discharge of industrial waste water.
Detailed Description
A resin desorbent comprises an acid cleaning solution I, a saline-alkali + organic solvent cleaning solution, a saline-alkali cleaning solution and an acid cleaning solution II, wherein the acid cleaning solution I is 1.5-3BV of (2-8) wt% hydrochloric acid, the saline-alkali + organic solvent cleaning solution is 0.5-1BV of (2-5) wt% NaOH + (8-12) wt% NaCl + (20-30) wt% organic solvent solution, the saline-alkali cleaning solution is 2-4BV of (2-5) wt% NaOH + (8-12) wt% NaCl solution, and the acid cleaning solution II is 0.5-1.5BV of (2-3) wt% hydrochloric acid.
Preferably, the mass percentage of the hydrochloric acid in the acid cleaning solution II is less than that of the hydrochloric acid in the acid cleaning solution I.
The desorption method adopting the resin desorption agent comprises the following steps: transferring the resin in the adsorption tank into a desorption tank, and carrying out the following steps in sequence: acid cleaning is carried out firstly, saline alkali + organic solvent cleaning is carried out, saline alkali cleaning is carried out, and acid cleaning is carried out secondly.
Preferably, an air-entrained backwash is performed to loosen the resin before the resin in the adsorption tank is transferred.
Preferably, the first acid wash is: adopting (2-8) wt% hydrochloric acid 1.5-3BV, temperature 52-58 deg.C, cleaning in two steps, half amount of each step, soaking in the first step for not less than 1 hr, stirring with compressed air, and washing with deionized water.
The saline-alkali + organic solvent cleaning is as follows: (2-5) NaOH + (8-12) NaCl + (20-30) wt% organic solvent solution 0.5-1BV, temperature 52-58 deg.C, soaking for 2 hours, then rinsing 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, the temperature is 52-58 ℃, the cleaning is carried out in three steps, the using amount of one sixth of the first two steps is one, the soaking time in the first step is not less than 2 hours, and then the cleaning is carried out by deionized water and the cleaning is carried out; in the second step, the soaking time is not less than 2 hours, the stirring is carried out by compressed air in the soaking process, and after the soaking is finished, the washing is carried out by deionized water and the water is drained; and thirdly, using two thirds of the dosage, and then washing with deionized water.
The second acid cleaning step is as follows: (2-3) 0.5-1.5BV of hydrochloric acid, normal temperature, and finally washing with deionized water.
Preferably, the method further comprises the step of treating the elution waste liquid by adopting a wet oxidation process, wherein the wet oxidation process comprises the following steps: adjusting pH of the elution waste liquid to 2-4 with sulfuric acid, adding hydrogen peroxide according to the concentration of 2-5%, and mixing uniformly; heating the reaction tower to 145-150 ℃ by using steam, and then sending the prepared stock solution into the reaction tower, wherein the effective retention time of the stock solution in the reaction tower is 1.5-2 h.
After desorption, the resin was transferred back to the adsorption tank.
Specifically, the desorption can be carried out using the specific steps in table 1.
TABLE 1
Figure RE-GDA0003699516470000041
Figure RE-GDA0003699516470000051
Along with the extension of operating time, conventional jar interior desorption mode is after through the manifold cycles, the adsorption performance of resin can fall to below 80% of initial adsorption performance usually, jar interior desorption is difficult to promote the adsorption performance of resin again, the desorption degree that adopts the desorption method in this application can show improvement resin, adopt the concrete step in table 1 to carry out the desorption back, the adsorption performance of resin can be recovered to more than 90% by below 80% of original adsorption performance, the desorption effect obviously promotes, thereby can reduce the use cost of resin by a wide margin.
Optionally, the elution waste liquid is treated by a wet oxidation process, wherein the wet oxidation process comprises the following steps: adjusting pH of the elution waste liquid to 2-4 with sulfuric acid, adding hydrogen peroxide according to the concentration of 2-5%, and mixing uniformly; heating the reaction tower to 145-150 ℃ by using steam, and then sending the prepared stock solution into the reaction tower, wherein the effective retention time of the stock solution in the reaction tower is 1.5-2 h.
The results of the elution waste liquid after the wet oxidation process are shown in table 2. As can be seen from Table 2, the removal rate of the elution waste liquid is more than 80%, and the maximum removal rate can reach 92%, so that the organic matters in the elution waste liquid can be efficiently removed, and the standard discharge of the waste liquid is realized.
TABLE 2
Figure RE-GDA0003699516470000052
Figure RE-GDA0003699516470000061
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 for convenience in describing and simplifying the description, and do not indicate or imply that the device or element so referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the invention. Furthermore, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In the description of the present invention, reference to the description of the terms "one embodiment," "some embodiments," "an illustrative embodiment," "an example," "a specific example," or "some examples" or the like 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, the schematic representations of the terms used above do not necessarily 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.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.

Claims (10)

1. A resin desorbent is characterized by comprising a first acid cleaning solution, a first saline-alkali + organic solvent cleaning solution, a second saline-alkali cleaning solution and a second acid cleaning solution, wherein the first acid cleaning solution is (2-8) wt% of hydrochloric acid 1.5-3BV, the saline-alkali + organic solvent cleaning solution is (2-5) wt% of NaOH + (8-12) wt% of NaCl + (20-30) wt% of organic solvent solution 0.5-1BV, the saline-alkali cleaning solution is (2-5) wt% of NaOH + (8-12) wt% of NaCl solution 2-4BV, and the second acid cleaning solution is (2-3) wt% of hydrochloric acid 0.5-1.5 BV.
2. The resin desorbent of claim 1 wherein the mass percent of the hydrochloric acid in the second acid cleaning solution is less than the mass percent of the hydrochloric acid in the first acid cleaning solution.
3. The resin desorbent of claim 1 wherein the organic solvent is an organic acid, an organic alcohol, or a combination thereof.
4. The resin desorbent of claim 3 wherein the organic acid is oxalic acid, acetic acid or citric acid; the organic alcohol is methanol or isopropanol.
5. The desorption method using the resin desorbent of claims 1 to 4, which comprises: transferring the resin in the adsorption tank into a desorption tank, and carrying out the following steps in sequence: acid cleaning is carried out firstly, saline alkali + organic solvent cleaning is carried out, saline alkali cleaning is carried out, and acid cleaning is carried out secondly.
6. The method of claim 5, wherein the first acid wash is: adopting (2-8)% hydrochloric acid 1.5-3BV, temperature 52-58 deg.C, cleaning in two steps, half amount of each step, soaking in the first step for not less than 1 hr, stirring with compressed air, and washing with deionized water.
7. The method according to claim 5, characterized in that the saline-alkali + organic solvent washing is: 2-5% NaOH + (8-12)% NaCl + (20-30)% organic solvent solution 0.5-1BV at 52-58 deg.C, soaking for 2 hours, and washing with deionized water.
8. The method according to claim 6, characterized in that the saline-alkali cleaning is: 2-4BV of (2-5)% NaOH + (8-12)% NaCl solution at 52-58 deg.C, three-step cleaning, one sixth of the first step, soaking for no less than 2 hr, washing with deionized water, and draining; in the second step, the soaking time is not less than 2 hours, the stirring is carried out by compressed air in the soaking process, and after the soaking is finished, the washing is carried out by deionized water and the water is drained; and thirdly, using two thirds of the dosage, and then washing with deionized water.
9. The method of claim 5, wherein the acid wash two is: (2-3)% hydrochloric acid 0.5-1.5BV, normal temperature, finally washing with deionized water.
10. The method of claim 5, further comprising treating the elution waste stream with a wet oxidation process, the wet oxidation process comprising: adjusting pH of the elution waste liquid to 2-4 with sulfuric acid, adding hydrogen peroxide according to the concentration of 2-5%, and mixing uniformly; heating the reaction tower to 145-150 ℃ by using steam, and then sending the prepared stock solution into the reaction tower, wherein the effective retention time of the stock solution in the reaction tower is 1.5-2 h.
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Publication number Priority date Publication date Assignee Title
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
CN110237832A (en) * 2019-05-29 2019-09-17 江苏南大环保科技有限公司 A kind of regeneration method of coking tail water absorption 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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Publication number Priority date Publication date Assignee Title
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
CN110237832A (en) * 2019-05-29 2019-09-17 江苏南大环保科技有限公司 A kind of regeneration method of coking tail water absorption 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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Title
环境保护部宣传教育中心等编著: "《持久性有机污染物及其防治》", 30 November 2014, 中国环境科学出版社 *

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