CN111151307A - Regeneration method of ion exchange resin for refining caprolactam water solution - Google Patents
Regeneration method of ion exchange resin for refining caprolactam water solution Download PDFInfo
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- CN111151307A CN111151307A CN201911416658.XA CN201911416658A CN111151307A CN 111151307 A CN111151307 A CN 111151307A CN 201911416658 A CN201911416658 A CN 201911416658A CN 111151307 A CN111151307 A CN 111151307A
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- exchange resin
- ion exchange
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- aqueous
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- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 239000003456 ion exchange resin Substances 0.000 title claims abstract description 70
- 229920003303 ion-exchange polymer Polymers 0.000 title claims abstract description 70
- 238000011069 regeneration method Methods 0.000 title claims abstract description 66
- 238000007670 refining Methods 0.000 title claims abstract description 21
- AWSFEOSAIZJXLG-UHFFFAOYSA-N azepan-2-one;hydrate Chemical compound O.O=C1CCCCCN1 AWSFEOSAIZJXLG-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 239000011347 resin Substances 0.000 claims abstract description 65
- 229920005989 resin Polymers 0.000 claims abstract description 65
- 230000008929 regeneration Effects 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 50
- 150000002500 ions Chemical class 0.000 claims abstract description 28
- 238000011001 backwashing Methods 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 239000012535 impurity Substances 0.000 claims abstract description 24
- 238000005406 washing Methods 0.000 claims abstract description 19
- 230000001172 regenerating effect Effects 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 92
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 75
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 44
- 239000003729 cation exchange resin Substances 0.000 claims description 36
- 238000003795 desorption Methods 0.000 claims description 29
- 239000003957 anion exchange resin Substances 0.000 claims description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 13
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 10
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 8
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 6
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 3
- 239000010865 sewage Substances 0.000 abstract description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 22
- 229910001410 inorganic ion Inorganic materials 0.000 description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 7
- 229910017604 nitric acid Inorganic materials 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000011010 flushing procedure Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- CHRJZRDFSQHIFI-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;styrene Chemical compound C=CC1=CC=CC=C1.C=CC1=CC=CC=C1C=C CHRJZRDFSQHIFI-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- -1 functional group cation Chemical class 0.000 description 1
- 238000007131 hydrochloric acid regeneration reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 229940127557 pharmaceutical product Drugs 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- 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
- B01J49/60—Cleaning or rinsing ion-exchange beds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
The invention discloses a regeneration method of ion exchange resin for refining caprolactam water solution, which comprises the following steps: (1) back washing the ineffective ion exchange resin by using an alcohol solution, and washing impurity ions attached to the surface of the resin; (2) resolving the ion exchange resin treated in the step (1) by using a resolving solution; (3) washing the ion exchange resin treated in the step (2) with water; (4) regenerating the ion exchange resin treated in the step (3) by using a regeneration liquid; (5) and (4) washing the ion exchange resin treated in the step (4) with water to obtain a regenerated ion exchange resin. The invention provides an economic and environment-friendly regeneration method, which not only obtains good regeneration effect, but also greatly reduces the sewage quantity and saves the cost of environment-friendly treatment.
Description
Technical Field
The invention relates to a regeneration method of ion exchange resin, in particular to a regeneration method of ion exchange resin for refining caprolactam water solution.
Background
Ion exchange resins are widely used in the production of chemical, biochemical and pharmaceutical products to extract and refine compounds. The repeated recycling of ion exchange resin is one of the main advantages of ion exchange resin in wide use in industrial production.
The regeneration of ion exchange resin is mainly directed to the process of introducing regeneration liquid into an ion exchanger filled with ion exchange resin to recover the ion exchange capacity of the resin. Usually, in order to achieve a better regeneration effect, the suspended substances on the resin are washed away by water, then the desorption solution is introduced, the desorption solution can remove the impurity ions adsorbed or firmly combined on the ion exchange resin, and finally the regeneration solution is introduced.
The ion exchange resin belongs to strong acid and strong base type styrene-divinylbenzene resin, the main functional group cation resin is toluene with a sulfonic acid group on the methylene, and the anion resin is toluene with a quaternary ammonium salt on the methylene.
Because of the high requirements of caprolactam refining on ion exchange resins, a strict procedure is set for the regeneration of resins for the refining of aqueous caprolactam solutions. Caprolactam production enterprises basically adopt the following steps: the anion exchange resin is firstly washed by dilute nitric acid and then regenerated by dilute caustic soda, and the cation exchange resin is firstly washed by dilute caustic soda and then regenerated by dilute nitric acid solution. The regeneration with nitric acid and caustic soda consumes a large amount of nitric acid and caustic soda, is high in cost, generates a large amount of wastewater containing acid and base, has a large wastewater treatment capacity, and is not environment-friendly.
For example, patent CN102728415A discloses a regeneration method of ion exchange resin for refining caprolactam water solution, wherein the regeneration method is one of the following combinations of steps (1) a, b; (2) a, c, b; (3) a, b, c; (4) a, d, c, b; (5) a, b, d, c; wherein: step a, draining a caprolactam water solution in the resin, and then cleaning the caprolactam in the resin by using process water; b, desorbing and regenerating the anion exchange resin and the cation exchange resin by using a methanol water solution with the mass concentration of 50-100%, and cleaning the resins by using process water; step c, the anion exchange resin is regenerated by dilute sodium hydroxide aqueous solution, the cation exchange resin is regenerated by dilute nitric acid, and then the resin is cleaned by process water; and d, regenerating the cation exchange resin by using a dilute sodium hydroxide aqueous solution, regenerating the anion exchange resin by using dilute nitric acid, and cleaning the resin by using process water. The invention adopts a mode of combining methanol regeneration and traditional acid-base regeneration, thereby reducing the usage amount of nitric acid and caustic soda. The disadvantages are as follows:
(1) a large amount of 50-100 wt% methanol solution is needed, so that the production cost is high;
(2) the regeneration time is long, and the whole regeneration period is as long as more than 15 hours;
(3) the process water has large usage amount, generates a large amount of waste water and brings heavy environmental protection pressure to enterprises
Disclosure of Invention
The invention aims to provide a method for regenerating ion exchange resin for refining caprolactam water solution, which has low cost, environmental protection and high efficiency aiming at the defects of the prior art.
In order to solve the technical problems, the invention is realized by the following technical scheme: a regeneration method of ion exchange resin for refining caprolactam water solution comprises the following steps:
(1) back washing the ineffective ion exchange resin by using an alcohol solution, washing impurity ions attached to the surface of the resin, and finishing the back washing when the caprolactam content of back washing effluent is less than or equal to 0.5 wt%;
(2) resolving the ion exchange resin treated in the step (1) by using a resolving solution to remove impurity ions adsorbed or fixed on the resin;
(3) washing the ion exchange resin treated in the step (2) with water to remove the residual desorption solution on the resin;
(4) regenerating the ion exchange resin treated in the step (3) by using a regeneration liquid to recover the regeneration capacity of the ion exchange resin;
(5) and (4) washing the ion exchange resin treated in the step (4) with water to remove the regeneration liquid remained on the resin, so as to obtain the regenerated ion exchange resin.
In a preferred embodiment of the present invention, the ion exchange resin is a cation exchange resin or an anion exchange resin.
In a preferred embodiment of the present invention, the alcohol solution is one of tert-butanol and propanol.
In a preferred embodiment of the present invention, the concentration of the alcohol solution is 5 to 10 wt% (wt%, mass%).
In a preferred embodiment of the present invention, when the ion exchange resin is a cation exchange resin, the desorption solution is at least one of an aqueous potassium hydroxide solution, an aqueous sodium hydroxide solution and an aqueous calcium hydroxide solution, and the regeneration solution is at least one of sulfuric acid, hydrochloric acid and hydrobromic acid.
In a preferred embodiment of the present invention, when the ion exchange resin is an anion exchange resin, the desorption solution is one of sulfuric acid, hydrochloric acid and hydrobromic acid, and the regeneration solution is at least one of an aqueous potassium hydroxide solution, an aqueous sodium hydroxide solution and an aqueous calcium hydroxide solution.
In a preferred embodiment of the present invention, the concentration of the sulfuric acid, hydrochloric acid, and hydrobromic acid is 2 to 8 wt%, and the concentration of the potassium hydroxide aqueous solution, sodium hydroxide aqueous solution, and calcium hydroxide aqueous solution is 3 to 9 wt%.
As a preferred embodiment of the invention, the flow rate of the analysis solution in the step (2) is 0.5-4.5 BV (BV refers to the volume of the resin bed layer), and the introduction time is 0.5-4 h.
As a preferred embodiment of the invention, the flow rate of the water in the step (3) and the step (5) is 0.5-3 BV, and the feeding time is 0.5-3.5 h.
As a preferred embodiment of the invention, the flow rate of the regeneration liquid in the step (4) is 0.5-4.5 BV, and the feeding time is 0.5-4 h.
The regeneration method of ion exchange resin for refining caprolactam water solution comprises the following steps of firstly, back washing by adopting an alcohol solution to wash off organic impurities and inorganic ions attached to the surface of the resin; then introducing a resolving liquid to remove impurity ions adsorbed or fixed on the resin; then washing with water to prevent resin poisoning failure caused by acid-base neutralization reaction; then introducing a regeneration liquid to recover the regeneration capacity of the ion exchange resin; and finally, washing with water. The invention provides an economic and environment-friendly regeneration method, which not only obtains good regeneration effect, but also greatly reduces the cost
The sewage quantity is reduced, and the cost of environmental protection treatment is saved. The method of the invention is suitable for any type of resin for refining caprolactam water solution.
Compared with the prior art, the invention has the advantages that:
1. the cost is low, only a small amount of 5-10 wt% alcohol solution is needed, and the production cost is greatly reduced;
2. the efficiency is high, the regeneration time is short, the whole regeneration period is less than 10 hours, and the regeneration period is shortened by one third compared with the prior art;
3. green and environment-friendly, remarkably reduces the using amount of water and further greatly reduces the amount of wastewater.
Detailed Description
The present invention will be described in further detail with reference to examples.
Regeneration method of ion exchange resin for refining caprolactam water solution
Example 1
(1) Introducing a tertiary butanol solution with the concentration of 5 wt% from the bottom of a cation exchange resin exchanger filled with the failed cation exchange resin, performing back washing on the cation exchange resin to ensure that a resin bed layer is fully crushed, and simultaneously washing organic impurities and inorganic ions attached to the surface of the resin, wherein when the caprolactam content of back washing effluent is less than or equal to 0.5 wt%, the back washing can be considered to be completed;
(2) introducing 4 wt% of sodium hydroxide solution into the cation exchange resin exchanger treated in the step (1) in a downstream mode, removing impurity ions adsorbed or fixed on the resin, wherein the flow rate of the sodium hydroxide solution is 2BV, and the introduction time is 3 h;
(3) introducing water into the cation exchange resin exchanger treated in the step (2) to remove the residual desorption solution on the resin, wherein the water flow is 1BV, and the introduction time is 2 h;
(4) introducing 5 wt% of dilute sulfuric acid regeneration liquid into the cation exchange resin exchanger treated in the step (3) to recover the regeneration capacity of the ion exchange resin, wherein the flow rate of the regeneration liquid is 2BV, and the introduction time is 3 h;
(5) and (4) introducing water into the cation exchange resin exchanger treated in the step (4), wherein the water flow rate is 0.5BV, and the introduction time is 1h, and removing the residual analysis solution on the resin to obtain the regenerated ion exchange resin.
Example 2
(1) Introducing a 5 wt% tert-butyl alcohol solution into the bottom of an anion exchange resin exchanger filled with the failed anion exchange resin, performing back washing on the anion exchange resin to fully crush a resin bed layer, and simultaneously washing organic impurities and inorganic ions attached to the surface of the resin, wherein when the caprolactam content of back washing effluent is less than or equal to 0.5 wt%, the back washing is considered to be completed;
(2) introducing a hydrobromic acid desorption solution with the weight percent of 5 into the anion exchange resin exchanger treated in the step (1) in a forward flow mode, removing impurity ions adsorbed or fixed on the resin, wherein the flow rate of the hydrobromic acid desorption solution is 1BV, and the introduction time is 2 h;
(3) introducing water into the ion exchanger treated in the step (2) to remove the residual desorption solution on the resin, wherein the water flow is 1BV, and the introduction time is 1.5 h;
(4) introducing 4 wt% of sodium hydroxide regeneration liquid into the ion exchanger treated in the step (3),
the regeneration capacity of the ion exchange resin is recovered, the flow rate of the regeneration liquid is 2BV, and the introduction time is 3 h.
(5) And (4) introducing water into the ion exchanger treated in the step (4) to remove the residual desorption solution on the resin, wherein the water flow is 2BV, and the introduction time is 2h to obtain the regenerated ion exchange resin.
Example 3
(1) Introducing a propanol solution of 6 percent from the bottom of a cation exchange resin exchanger filled with the failed cation exchange resin, performing back washing on the cation exchange resin to fully crush a resin bed layer, and simultaneously washing organic impurities and inorganic ions attached to the surface of the resin, wherein when the caprolactam content of back washing effluent is less than or equal to 0.5 weight percent, the back washing can be regarded as being completed;
(2) introducing 6 wt% of sodium hydroxide solution into the cation exchange resin exchanger treated in the step (1) in a downstream mode, removing impurity ions adsorbed or fixed on the resin, wherein the flow rate of the sodium hydroxide solution is 3BV, and the introduction time is 1.5 h;
(3) introducing water into the cation exchange resin exchanger treated in the step (2) to remove the desorption solution remained on the resin, wherein the water flow is 2.5BV, and the introduction time is 1.5 h;
(4) introducing 6 wt% hydrobromic acid into the cation exchange resin exchanger treated in the step (3)
The regeneration liquid recovers the regeneration capacity of the ion exchange resin, the flow rate of the regeneration liquid is 3BV, and the charging time is 1.5 h;
(5) and (4) introducing water into the cation exchange resin exchanger treated in the step (4) to remove the residual desorption solution on the resin, wherein the water flow is 0.5BV, and the introduction time is 2.5h to obtain the regenerated ion exchange resin.
Example 4
(1) Introducing 7 wt% of propanol solution from the bottom of an anion exchange resin exchanger filled with the ineffective anion exchange resin, performing back flushing on the anion exchange resin to fully crush a resin bed layer, and simultaneously washing organic impurities and inorganic ions attached to the surface of the resin, wherein when the caprolactam content of back-flushed effluent is less than or equal to 0.5 wt%, the back flushing can be regarded as being completed;
(2) introducing 6 wt% hydrobromic acid desorption solution into the anion exchange resin exchanger treated in the step (1) in a concurrent flow manner, removing impurity ions adsorbed or fixed on the resin, wherein the flow rate of the hydrobromic acid desorption solution is 0.5BV, and the introduction time is 3.5 h;
(3) introducing water into the ion exchanger treated in the step (2) to remove the residual desorption solution on the resin, wherein the water flow is 1.5BV, and the introduction time is 2 h;
(4) introducing 6 wt% of sodium hydroxide regeneration liquid into the ion exchanger treated in the step (3) to recover the regeneration capacity of the ion exchange resin, wherein the flow rate of the regeneration liquid is 0.5BV, and the introduction time is 2.5 h;
(5) and (4) introducing water into the ion exchanger treated in the step (4) to remove the residual desorption solution on the resin, wherein the water flow is 3BV, and the introduction time is 1h to obtain the regenerated ion exchange resin.
Example 5
(1) Introducing 8% propanol solution from the bottom of a cation exchange resin exchanger filled with the failed cation exchange resin, performing back washing on the cation exchange resin to fully crush a resin bed layer, and simultaneously washing organic impurities and inorganic ions attached to the surface of the resin, wherein when the caprolactam content of back washing effluent is less than or equal to 0.5 wt%, the back washing can be regarded as being completed;
(2) introducing 6 wt% of sodium hydroxide solution into the cation exchange resin exchanger treated in the step (1) in a downstream mode, removing impurity ions adsorbed or fixed on the resin, wherein the flow rate of the sodium hydroxide solution is 1.5BV, and the introduction time is 2.5 h;
(3) introducing water into the cation exchange resin exchanger treated in the step (2) to remove the residual desorption solution on the resin, wherein the water flow is 0.5BV, and the introduction time is 2.5 h;
(4) introducing 7 wt% of hydrochloric acid regeneration liquid into the cation exchange resin exchanger treated in the step (3) to recover the regeneration capacity of the ion exchange resin, wherein the flow rate of the regeneration liquid is 1.5BV, and the introduction time is 3 h;
(5) and (4) introducing water into the cation exchange resin exchanger treated in the step (4) to remove the residual desorption solution on the resin, wherein the water flow is 2BV, and the introduction time is 1.5h to obtain the regenerated ion exchange resin.
Example 6
(1) Introducing a propanol solution with the concentration of 6 wt% from the bottom of an anion exchange resin exchanger filled with the ineffective anion exchange resin, performing back washing on the anion exchange resin to ensure that a resin bed layer is fully crushed, and simultaneously washing organic impurities and inorganic ions attached to the surface of the resin, wherein when the caprolactam content of back washing effluent is less than or equal to 0.5 wt%, the back washing can be considered to be completed;
(2) introducing 7 wt% dilute hydrochloric acid solution into the anion exchange resin exchanger treated in the step (1) in a downstream mode, removing impurity ions adsorbed or fixed on the resin, wherein the flow rate of the dilute sulfuric acid solution is 2.5BV, and the introduction time is 2.5 h;
(3) introducing water into the ion exchanger treated in the step (2) to remove the residual desorption solution on the resin, wherein the water flow is 1.5BV, and the introduction time is 2.5 h;
(4) introducing 6 wt% of sodium hydroxide regeneration liquid into the ion exchanger treated in the step (3) to recover the regeneration capacity of the ion exchange resin, wherein the flow rate of the regeneration liquid is 2.5BV, and the introduction time is 1.5h
(5) And (4) introducing water into the ion exchanger treated in the step (4) to remove the residual desorption solution on the resin, wherein the water flow is 2.5BV, and the introduction time is 1.5h, so as to obtain the regenerated ion exchange resin.
Example 7
(1) Introducing 7% of propanol solution from the bottom of a cation exchange resin exchanger filled with the failed cation exchange resin, performing back washing on the cation exchange resin to fully crush a resin bed layer, and simultaneously washing organic impurities and inorganic ions attached to the surface of the resin, wherein when the caprolactam content of back washing effluent is less than or equal to 0.5 wt%, the back washing can be regarded as being completed;
(2) introducing 7 wt% of sodium hydroxide solution into the cation exchange resin exchanger treated in the step (1) in a downstream mode, removing impurity ions adsorbed or fixed on the resin, wherein the flow rate of the sodium hydroxide solution is 1.5BV, and the introduction time is 2.5 h;
(3) introducing water into the cation exchange resin exchanger treated in the step (2) to remove the residual desorption solution on the resin, wherein the water flow is 2.5BV, and the introduction time is 0.5 h;
(4) introducing 3 wt% dilute sulfuric acid regeneration liquid into the cation exchange resin exchanger treated in the step (3) to recover the regeneration capacity of the ion exchange resin, wherein the flow rate of the regeneration liquid is 0.5BV, and the introduction time is 2.5h
(5) And (4) introducing water into the cation exchange resin exchanger treated in the step (4) to remove the residual desorption solution on the resin, wherein the water flow is 1.5BV, and the introduction time is 1.5h to obtain the regenerated ion exchange resin.
Example 8
(1) Introducing 8 wt% of propanol solution from the bottom of an anion exchange resin exchanger filled with the ineffective anion exchange resin, performing back flushing on the anion exchange resin to fully crush a resin bed layer, and simultaneously washing organic impurities and inorganic ions attached to the surface of the resin, wherein when the caprolactam content of back-flushed effluent is less than or equal to 0.5 wt%, the back flushing can be regarded as being completed;
(2) introducing 3 wt% dilute sulfuric acid solution into the anion exchange resin exchanger treated in the step (1) in a downstream mode, removing impurity ions adsorbed or fixed on the resin, wherein the flow rate of the dilute sulfuric acid solution is 0.5BV, and the introduction time is 3 h;
(3) introducing water into the ion exchanger treated in the step (2), removing the residual desorption solution on the resin, wherein the water flow is 1BV, and the introduction time is 1 h;
(4) introducing 7 wt% of sodium hydroxide regeneration liquid into the ion exchanger treated in the step (3) to recover the regeneration capacity of the ion exchange resin, wherein the flow rate of the regeneration liquid is 1.5BV, and the introduction time is 1.5h
(5) And (4) introducing water into the ion exchanger treated in the step (4) to remove the residual desorption solution on the resin, wherein the water flow is 1BV, and the introduction time is 3h to obtain the regenerated ion exchange resin.
Claims (10)
1. A regeneration method of ion exchange resin for refining caprolactam water solution is characterized by comprising the following steps:
(1) back washing the ineffective ion exchange resin by using an alcohol solution, washing impurity ions attached to the surface of the resin, and finishing the back washing when the caprolactam content of back washing effluent is less than or equal to 0.5 wt%;
(2) resolving the ion exchange resin treated in the step (1) by using a resolving solution to remove impurity ions adsorbed or fixed on the resin;
(3) washing the ion exchange resin treated in the step (2) with water to remove the residual desorption solution on the resin;
(4) regenerating the ion exchange resin treated in the step (3) by using a regeneration liquid to recover the regeneration capacity of the ion exchange resin;
(5) and (4) washing the ion exchange resin treated in the step (4) with water to remove the regeneration liquid remained on the resin, so as to obtain the regenerated ion exchange resin.
2. The method for regenerating an ion exchange resin for refining an aqueous caprolactam solution according to claim 1, wherein the ion exchange resin is a cation exchange resin or an anion exchange resin.
3. The method for regenerating an ion exchange resin for refining an aqueous caprolactam solution according to claim 1, wherein the alcohol solution is one of t-butanol and propanol.
4. The method for regenerating an ion exchange resin for refining an aqueous caprolactam solution according to claim 1, wherein the concentration of the alcohol solution is 5 to 10 wt%.
5. The method of regenerating an ion exchange resin for refining an aqueous caprolactam solution according to claim 2, wherein when the ion exchange resin is a cation exchange resin, the desorption solution is at least one of an aqueous potassium hydroxide solution, an aqueous sodium hydroxide solution and an aqueous calcium hydroxide solution, and the regeneration solution is at least one of sulfuric acid, hydrochloric acid and hydrobromic acid.
6. The method of claim 2, wherein when the ion exchange resin is an anion exchange resin, the desorption solution is one of sulfuric acid, hydrochloric acid and hydrobromic acid, and the regeneration solution is at least one of an aqueous potassium hydroxide solution, an aqueous sodium hydroxide solution and an aqueous calcium hydroxide solution.
7. The method for regenerating an ion exchange resin for refining an aqueous caprolactam solution according to claim 5 or 6, wherein the concentration of the sulfuric acid, the hydrochloric acid, and the hydrobromic acid is 2 to 8 wt%, and the concentration of the hydrogen and the oxygen is 2 to 8 wt%
The concentration of the potassium hydroxide aqueous solution, the sodium hydroxide aqueous solution and the calcium hydroxide aqueous solution is 3-9 wt%.
8. The method for regenerating an ion exchange resin for refining an aqueous caprolactam solution according to claim 1, wherein the flow rate of the desorption solution in the step (2) is 0.5 to 4.5BV, and the time for passing the desorption solution is 0.5 to 4 hours.
9. The method for regenerating an ion exchange resin for refining an aqueous caprolactam solution according to claim 1, wherein the flow rate of the water in the step (3) and the step (5) is 0.5 to 3BV, and the time for introducing the water is 0.5 to 3.5 hours.
10. The method for regenerating an ion exchange resin for refining an aqueous caprolactam solution according to claim 1, wherein the flow rate of the regeneration liquid in the step (4) is 0.5 to 4.5BV, and the feeding time is 0.5 to 4 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911416658.XA CN111151307A (en) | 2019-12-31 | 2019-12-31 | Regeneration method of ion exchange resin for refining caprolactam water solution |
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| CN115957811A (en) * | 2023-01-12 | 2023-04-14 | 中国天辰工程有限公司 | In-situ regeneration method of liquid phase Beckmann rearrangement catalyst |
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