CN112316989B - Regeneration method of ion exchange resin - Google Patents
Regeneration method of ion exchange resin Download PDFInfo
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- CN112316989B CN112316989B CN202011134277.5A CN202011134277A CN112316989B CN 112316989 B CN112316989 B CN 112316989B CN 202011134277 A CN202011134277 A CN 202011134277A CN 112316989 B CN112316989 B CN 112316989B
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- 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
Abstract
The invention provides a regeneration method of ion exchange resin, which comprises the following steps: (1) Washing the resin with water for the first time to obtain resin with loose particles; (2) Washing the resin obtained in the step (1) with hydrochloric acid, and soaking to obtain H + A resin; (3) The obtained H + And washing the resin with primary saline water, introducing a mixed solution of the primary saline water and alkali liquor, and washing with the primary saline water to obtain the regenerated resin. The method is simple, the dosage of the regenerant is small, the cost is low, the regeneration efficiency of the obtained resin is high, the service life is long, and the materials can be recycled.
Description
Technical Field
The invention belongs to the field of resin regeneration, and particularly relates to a regeneration method of ion exchange resin.
Background
Ion exchange is a common process in refining and extracting processes, the ion exchange reaches a certain degree, the adsorption capacity of resin reaches saturation, and acid and alkali are required to be used for regeneration to obtain the exchange capacity again. The existing ion exchange resin regeneration process is to pass acid with a certain concentration through a cation resin column and alkali through an anion resin column, and acid-alkali liquid flowing out of the resin column is directly discharged into a sewage treatment plant without being recycled. In the existing ion exchange resin regeneration process, although hydrochloric acid is a good regenerant, the cost is high, the regeneration efficiency is low, and according to statistics, a large-scale pharmaceutical factory only recovers cation exchange resin and consumes 500 tons of hydrochloric acid per month, so that the reduction of the consumption of the regenerant is a key problem of reducing the product cost.
In short, the existing ion exchange resin regeneration process has the problems of environmental pollution, economy, large using amount of regenerant, low regeneration efficiency and poor effect, and seriously affects the service life of the resin, so that the development of the regeneration process of the ion exchange resin, which is economical, environment-friendly, high in regeneration efficiency and long in service life of the resin, is urgently needed.
Disclosure of Invention
The invention aims to provide a method for regenerating ion exchange resin, which has the advantages of small using amount of a regenerant, high resin regeneration efficiency, long service life and low cost.
The potash industry requires salting and two brine refinements of KCl solid feedstock prior to electrolysis of KCl: firstly, crude brine with the salt dissolving ratio of about 320g/L is prepared, calcium, magnesium, sulfate radical and other ions in the crude brine are removed mainly by adding some refining agents through the operation procedures of clarification, filtration and the like in the primary brine refining, and the calcium, magnesium and other ions remained in the primary brine are generally adsorbed by adopting cationic resin in the secondary brine refining. When the resin needs to be regenerated after being used for a period of time, the traditional resin regeneration process needs a large amount of regenerants, has low regeneration efficiency and poor effect, and seriously influences the service life of the resin. In the invention, the inventor develops a novel regeneration process of the ion exchange resin, which can not only reduce the using amount of the regenerant, but also improve the regeneration efficiency of the resin. The invention provides a method for preparing a compound H + Substitution of resin for Na + Resin or K + A resin-in-resin process, said regenerative displacement process comprising the steps of:
(1) Will H + Washing the resin with primary saline;
(2) Then introducing a mixed solution of primary saline water and alkali liquor for washing;
(3) Finally, saline water is introduced for washing once again;
the primary brine is NaCl or KCl solution, and the alkali liquor is sodium hydroxide aqueous solution or potassium hydroxide aqueous solution.
The alkali liquor is obtained by electrolysis, and the method uses primary brine and the alkali liquor obtained by electrolysis as regenerants and is matched with specific regeneration process steps, so that the resin loss rate and the cost can be reduced, and the calcium and magnesium ion removal rate can be improved; in the step (2), the primary brine and the alkali liquor can be mixed and then the flushing resin is introduced, or the flushing resin can be introduced at the same time.
In a particular embodiment of the invention, the concentration of the primary brine is between 310 and 330g/L, preferably 320g/L, with a calcium and magnesium ion content of 0.8ppm.
In a specific embodiment of the invention, the mass fraction of the alkali liquor is 25% -35%, preferably 30%.
The alkali liquor is obtained by an electrolysis process.
In a specific embodiment of the invention, the primary brine is introduced at a flow rate of 1.9m per ton of resin 3 /h～2.1m 3 H, preferably 2m 3 H, alkali liquor is introduced at a flow rate of 0.06m 3 /h～0.09m 3 H, preferably 0.08m 3 /h；
The resin dosage in the embodiment of the invention is 8 tons, namely the flow of the resin introduced into the primary brine is 15m 3 /h～17m 3 H, preferably 16m 3 H, alkali liquor is introduced at a flow rate of 0.5m 3 /h～0.7m 3 H, preferably 0.6m 3 /h。
Further, in the step (2), the solution is washed until the pH value is 10-12.
The invention also provides a regeneration method of the cation exchange resin, which comprises the following steps:
s1, washing resin with pure water;
s2, replacing the resin obtained in the step S1 with hydrochloric acid to obtain H + A resin;
s3, mixing H according to the method + Replacing the resin to obtain regenerated resin;
in a specific embodiment of the present invention, the washing in S1 is a forward washing followed by a backwashing.
Further, the flow of pure water is 1.75m per ton of resin 3 /h～2m 3 H, preferably 1.9m 3 /h；
The resin dosage in the embodiment of the invention is 8 tons, namely the resin flow of pure water is 14m 3 /h～16m 3 H, preferably 15m 3 /h。
The time of the forward washing in the washing is 1.3 h-2 h, preferably 1.5h; the backwashing time is 1.3 h-2 h, preferably 2h.
In a specific embodiment of the present invention, the pH of the hydrochloric acid in step S2 is 1 to 2;
furthermore, the replacement by hydrochloric acid is that the hydrochloric acid is firstly used for direct washing, and then the hydrochloric acid is used for soaking;
further, the time of the hydrochloric acid forward washing is 1.3 h-2 h, and preferably 2h.
Further, the soaking time is 1.5 to 2.1 hours, preferably 2 hours.
In the embodiment of the invention, the method further comprises a step of replacing the residual hydrochloric acid with pure water before the step S3;
further, the pure water replacement is a forward washing with pure water;
further, the pH of the pure water is 5-7, and the time is 1.3-2 h, preferably 2h.
The regeneration water and the solution in all regeneration steps are recycled to the salt dissolving stage, and primary brine is obtained again, so that the materials can be recycled, and the loss of raw materials is reduced. The invention has the following beneficial effects:
(1) The method is simple, low in cost and small in regenerant consumption, the removal rate of calcium and magnesium ions in the resin is higher than 99%, the regeneration efficiency is high, the loss rate of the resin is lower than 0.6%, and the service life is prolonged.
(2) The regeneration water and the solution in all regeneration steps are recycled to the salt dissolving stage to obtain primary brine again, so that the materials are recycled, the loss of raw materials is reduced, and the method is economic and environment-friendly.
Detailed Description
The technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are some, not all embodiments of the present invention. Other embodiments, which can be obtained by persons skilled in the art without any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The cation resin needing regeneration in the embodiment of the invention is strong acid styrene cation resin used for secondary brine refining in potash industry, calcium and magnesium ions in the resin are saturated and then sent to the resin for regeneration, the specification of a resin tower adopted in the embodiment is phi 2400 multiplied by 5984mm, the height of the resin layer is 1.4m, and the total amount of dry resin is 8 tons.
The primary brine used in the embodiment is a KCl aqueous solution with the mass fraction of 320g/L, wherein the content of calcium and magnesium ions is 0.8ppm; flow rate of pure water introduced into pipelineAt a flow rate of 15m 3 H, the flow of primary brine in the pipeline is 16m 3 30% KOH introduction rate of 0.6m 3 /h。
Example 1
The cation resin is regenerated by adopting the following steps:
(1) The cationic resin was forward washed with pure water for 1.5h, and the remaining brine in the off-line column was displaced, and pure water was taken in from the top of the column.
(2) Backwashing for 2h by pure water, wherein the pure water enters from the bottom of the tower, resin particles are loosened, and small particles are taken away.
(3) Washing with hydrochloric acid for 2H, soaking with hydrochloric acid for 2H (pH is controlled at 1-2), regenerating resin, and allowing divalent metal ions to be adsorbed by H + By displacement to give H + And (3) resin.
(4) Washing with pure water for 2h, and controlling the pH value to be 5-7 to replace the residual hydrochloric acid in the tower with the pure water.
(5) Will become H + Replacement of the resin of (A) by K + Resin type: introducing primary brine only for 30min, mixing the primary brine with the electrolyzed 30% KOH solution for 60min until the pH is 10-12, and finally introducing primary brine only for 30min.
All the regenerated water and the solution in the regeneration step enter a recovery pit and are uniformly sent to a brine working section by a pump for salt dissolving.
Example 2
The cation resin is regenerated by adopting the following steps:
(1) The cationic resin was forward washed with pure water for 1.5h, and the remaining brine in the off-line column was displaced, and pure water was taken in from the top of the column.
(2) Backwashing for 2h by pure water, wherein the pure water enters from the bottom of the tower, resin particles are loosened, and small particles are taken away.
(3) Washing with hydrochloric acid for 2H, soaking with hydrochloric acid for 2H (pH is controlled at 1-2), regenerating resin, and allowing divalent metal ions to be adsorbed by H + By displacement to give H + And (3) resin.
(4) The column is washed with pure water for 2h, and the pH is controlled to be 5-7, so that the residual hydrochloric acid in the column is replaced by the pure water.
(5) Will become H + Replacement of the resin of (A) by K + Resin type: introducing primary brine for 60min, mixing the primary brine with the electrolyzed 30% KOH solution, introducing the mixture for 60min until the pH is 10-12, and finally introducing the primary brine for 30min.
All the regenerated water and the solution in the regeneration step enter a recovery pit and are uniformly sent to a brine working section by a pump for salt dissolving.
Example 3
The cation resin is regenerated by adopting the following steps:
(1) The cationic resin was forward washed with pure water for 1.5h, and the remaining brine in the off-line column was displaced, and pure water was taken in from the top of the column.
(2) And backwashing for 2h by using pure water, wherein the pure water enters from the bottom of the tower, resin particles are loosened, and small particles are taken away.
(3) Washing with hydrochloric acid for 2H, soaking with hydrochloric acid for 2H (pH is controlled at 1-2), regenerating resin, and allowing divalent metal ions to be adsorbed by H + By displacement to give H + And (3) resin.
(4) Washing with pure water for 2h, and controlling the pH value to be 5-7 to replace the residual hydrochloric acid in the tower with the pure water.
(5) Will become H + Replacement of the resin of (b) by K + Resin type: the first brine was first passed through for 30min, then the first brine was mixed with the 30% KOH solution obtained by electrolysis for 60min until the pH was 10 to 12, and finally the first brine was passed through for 60min.
All the regenerated water and the solution in the regeneration step enter a recovery pit and are uniformly sent to a brine working section by a pump for salt dissolving.
Example 4
The cation resin is regenerated by adopting the following steps:
(1) The cationic resin was forward washed with pure water for 1.5h, displacing the remaining brine in the off-line column, and pure water was fed from the top of the column.
(2) Backwashing for 2h by pure water, wherein the pure water enters from the bottom of the tower, resin particles are loosened, and small particles are taken away.
(3) Washing with hydrochloric acid for 2H, soaking with hydrochloric acid for 2H (pH is controlled at 1-2), regenerating resin, and allowing divalent metal ions to be adsorbed by H + Is displaced to give H + And (3) resin.
(4) The column is washed with pure water for 2h, and the pH is controlled to be 5-7, so that the residual hydrochloric acid in the column is replaced by the pure water.
(5) Will become H + Replacement of the resin of (b) by K + Resin type: the first brine was first introduced for 30min, then the first brine was mixed with the 30% KOH solution obtained by electrolysis for 30min to a pH of 10 to 12, and finally the first brine was introduced for 30min.
All the regenerated water and the solution in the regeneration step enter a recovery pit and are uniformly sent to a brine working section by a pump for salt dissolving.
Comparative example 1
(1) The cationic resin was forward washed with pure water for 1.5h, and the remaining brine in the off-line column was displaced, and pure water was taken in from the top of the column.
(2) Backwashing for 2h by pure water, wherein the pure water enters from the bottom of the tower, resin particles are loosened, and small particles are taken away.
(3) Washing with hydrochloric acid for 2H, soaking in hydrochloric acid for 2H (pH controlled at 1-2), regenerating resin, and allowing divalent metal ions to be adsorbed by H + By displacement to give H + And (3) resin.
(4) The column is washed with pure water for 2h, and the pH is controlled to be 5-7, so that the residual hydrochloric acid in the column is replaced by the pure water.
(5) Will become H + Replacement of the resin of (b) by K + Resin type: introducing primary saline water until the content of calcium and magnesium ions in the resin is not changed.
And (4) all the regenerated water and the solution in the regeneration step enter a recovery pit and are uniformly sent to a brine working section by a pump for salt dissolving.
Comparative example 2
(1) The cationic resin was forward washed with pure water for 1.5h, displacing the remaining brine in the off-line column, and pure water was fed from the top of the column.
(2) Backwashing for 2h by pure water, wherein the pure water enters from the bottom of the tower, resin particles are loosened, and small particles are taken away.
(3) Washing with hydrochloric acid for 2H, soaking in hydrochloric acid for 2H (pH controlled at 1-2), regenerating resin, and allowing divalent metal ions to be adsorbed by H + By displacement to give H + And (3) resin.
(4) Washing with pure water for 2h, and controlling the pH value to be 5-7 to replace the residual hydrochloric acid in the tower with the pure water.
(5) Passing the KOH solution 30% obtained by electrolysis through H + In the resin, the content of calcium and magnesium ions in the resin is not changed.
And (4) all the regenerated water and the solution in the regeneration step enter a recovery pit and are uniformly sent to a brine working section by a pump for salt dissolving.
Comparative example 3
(1) The cationic resin was forward washed with pure water for 1.5h, displacing the remaining brine in the off-line column, and pure water was fed from the top of the column.
(2) And backwashing for 2h by using pure water, wherein the pure water enters from the bottom of the tower, resin particles are loosened, and small particles are taken away.
(3) Washing with hydrochloric acid for 2H, soaking with hydrochloric acid for 2H (pH is controlled at 1-2), regenerating resin, and allowing divalent metal ions to be adsorbed by H + Is displaced to give H + And (3) resin.
(4) The column is washed with pure water for 2h, and the pH is controlled to be 5-7, so that the residual hydrochloric acid in the column is replaced by the pure water.
(5) H is to be + Mixing the resin with 30% KOH solution obtained by electrolysis with primary saline, introducing for 60min, controlling pH to 10-12, and introducing primary saline until the content of calcium and magnesium ions in the resin is not changed.
All the regenerated water and the solution in the regeneration step enter a recovery pit and are uniformly sent to a brine working section by a pump for salt dissolving.
The resin regeneration quality and the regenerant usage amount in examples 1 to 4 and comparative examples 1 to 3 were compared.
TABLE 1 comparison of resin regeneration quality and regenerant usage
As is clear from Table 1, examples 1 to 4 used 32 to 40m 3 Primary saline water, 0.3-0.6 m 3 30% KOH as a regenerant, the calcium-magnesium ion removal rate was 99.4% to 99.6%, the resin loss rate was 0.3% to 0.5%, and 80m was used in comparative example 1 3 When the primary brine of (2) is used as a regenerant,the calcium and magnesium ion removal rate is only 92.3 percent, the resin loss rate is 1.5 percent, and only 5m is used in the comparative example 2 3 30% KOH as a regenerant, the calcium-magnesium ion removal rate was 90.5% and the resin loss rate was 1.8%, compared with the case of comparative example 3 in which 70m KOH was used 3 Primary saline, 0.6m 3 30% KOH as a regenerant, the calcium-magnesium ion rejection rate was 91.2%, and the resin loss rate was 1.7%.
It can be seen that only the technical scheme in the embodiment is used, namely, after the primary saline water is firstly introduced to wash for 30-60 min in the replacement stage, 32-40 m is used 3 Primary saline water, 0.3-0.6 m 3 30% KOH as a regenerant, and then brine was introduced once when the pH was 10 to 12, thereby obtaining a resin having a high calcium and magnesium ion removal rate and a low resin loss rate.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (11)
1. A kind of device for removing H + Substitution of resin for Na + Resin or K + A method of forming a resin, said method comprising the steps of:
(1) Will H + Washing the resin with primary saline;
(2) Then, introducing a mixed solution of primary saline water and alkali liquor for flushing until the pH of the solution is 10 to 12, wherein the mass fraction of the alkali liquor is 25 to 35 percent;
(3) Finally, saline water is introduced for washing once again;
the primary saline is NaCl or KCl solution, and the alkali liquor is sodium hydroxide aqueous solution or potassium hydroxide aqueous solution; the flow of the primary brine introduced into each ton of resin is 1.9m 3 /h~2.1m 3 H; the flow rate of the alkali liquor is 0.06m 3 /h ~0.09m 3 /h。
2. The method as claimed in claim 1, wherein the concentration of the primary saline is 310 to 330g/L.
3. The method according to claim 1, characterized in that the mass fraction of the lye is 30%.
4. Replacement method according to claim 1, characterised in that the primary brine feed has a flow rate of 2m per ton of resin 3 H, the flow rate of the alkali liquor is 0.08m 3 /h。
5. A method for regenerating a cation exchange resin, comprising the steps of:
s1, washing resin with pure water;
s2, replacing the resin obtained in the step S1 with hydrochloric acid to obtain H + A resin;
s3, reacting H according to the method of any one of claims 1 to 4 + Replacing the resin to obtain regenerated resin;
the washing in the S1 is forward washing and back washing.
6. Regeneration process according to claim 5, characterised in that the pure water is introduced at a flow rate of 1.75m per ton of resin 3 /h~2m 3 /h；
The forward washing time in the washing process is 1.3h to 2h; the backwashing time is 1.3h to 2h.
7. The regeneration method according to claim 5, wherein the pH of the hydrochloric acid in step S2 is 1 to 2.
8. The regeneration method according to claim 7, wherein, in step S2,
the replacement by hydrochloric acid is that the hydrochloric acid is firstly used for direct washing, and then the hydrochloric acid is used for soaking.
9. The regeneration method of claim 7, wherein the hydrochloric acid forward washing time is 1.3 to 2h;
the soaking time is 1.5 to 2.1h.
10. The regeneration method according to claim 5, further comprising a step of replacing the remaining hydrochloric acid with pure water before step S3;
the pure water regeneration is a direct washing with pure water.
11. The regeneration method according to claim 9, wherein the pH of the pure water is 5 to 7, and the replacement time is 1.3 to 2h.
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