CN112808323A - Method for treating anion exchange resin by ammonia water - Google Patents
Method for treating anion exchange resin by ammonia water Download PDFInfo
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- CN112808323A CN112808323A CN202011574897.0A CN202011574897A CN112808323A CN 112808323 A CN112808323 A CN 112808323A CN 202011574897 A CN202011574897 A CN 202011574897A CN 112808323 A CN112808323 A CN 112808323A
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- China
- Prior art keywords
- exchange resin
- water
- anion exchange
- ammonia water
- ion exchange
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000003957 anion exchange resin Substances 0.000 title claims abstract description 43
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 235000011114 ammonium hydroxide Nutrition 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims abstract description 31
- 229910001868 water Inorganic materials 0.000 claims abstract description 25
- 238000005406 washing Methods 0.000 claims abstract description 19
- 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 claims abstract description 18
- 239000003456 ion exchange resin Substances 0.000 claims abstract description 18
- 229920003303 ion-exchange polymer Polymers 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 239000002244 precipitate Substances 0.000 claims abstract description 12
- 238000011001 backwashing Methods 0.000 claims abstract description 11
- 238000005342 ion exchange Methods 0.000 claims abstract description 9
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229910001863 barium hydroxide Inorganic materials 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 7
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910001626 barium chloride Inorganic materials 0.000 claims abstract description 6
- 230000001172 regenerating effect Effects 0.000 claims abstract description 4
- 239000012459 cleaning agent Substances 0.000 claims abstract description 3
- 239000012716 precipitator Substances 0.000 claims abstract description 3
- 239000012492 regenerant Substances 0.000 claims abstract description 3
- 239000011347 resin Substances 0.000 claims description 10
- 229920005989 resin Polymers 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 8
- 230000008929 regeneration Effects 0.000 claims description 8
- 238000011069 regeneration method Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000005056 compaction Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000000643 oven drying Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- 150000002500 ions Chemical class 0.000 claims description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 3
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 210000001035 gastrointestinal tract Anatomy 0.000 abstract 2
- 150000002632 lipids Chemical class 0.000 abstract 1
- 210000004400 mucous membrane Anatomy 0.000 abstract 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 21
- 238000000855 fermentation Methods 0.000 description 5
- 230000004151 fermentation Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 159000000007 calcium salts Chemical class 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 241000228245 Aspergillus niger Species 0.000 description 1
- 241001052560 Thallis Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 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
- B01J49/50—Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents
- B01J49/57—Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents for anionic exchangers
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
- C01F11/462—Sulfates of Sr or Ba
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
The invention discloses a method for treating anion exchange resin by ammonia water, which relates to the technical field of ammonia water treatment, and comprises the following steps of ammonia water, barium chloride and deionized water, wherein the ammonia water is used as a regenerant, the barium chloride is used as a precipitator, and the deionized water is used as a cleaning agent: and (3) introducing deionized water to the bottom of the ion exchange column filled with the anion exchange resin to carry out backwashing on the ion exchange resin. In the process of regenerating ion exchange resin, barium hydroxide is added to fully stir and stand with the water solution for washing the regenerated ion exchange resin to obtain barium sulfate precipitate and ammonia water, the barium sulfate can be applied to the field of medical treatment, the barium sulfate used in the radiological examination mainly utilizes the fact that the barium sulfate can absorb X rays in gastrointestinal tracts to enable the barium sulfate to develop, and the barium sulfate is insoluble in water and lipid and cannot be absorbed by gastrointestinal tract mucous membranes; the ammonia water can be repeatedly used, and the production cost is greatly reduced.
Description
Technical Field
The invention relates to the technical field of ammonia water treatment, in particular to a method for treating anion exchange resin by using ammonia water.
Background
Ion exchange resin is widely used in the production process of chemical and biochemical products for extracting and refining compounds, the ion exchange reaches a certain degree, the adsorption capacity of the resin is saturated, regeneration treatment is required, ions and other impurities adsorbed by the resin are eluted and removed by chemical agents to restore the original composition and performance, and the repeated regeneration and utilization of the ion exchange resin is one of the main advantages of the ion exchange resin in the industrial production.
China is a large country for citric acid production, the citric acid industry develops rapidly, the fermentation technology is in the world leading level particularly in the aspects of fermentation strains and production technology, but the downstream extraction technology is relatively backward, the aspergillus niger deep fermentation method is applied to citric acid production, the components of fermentation liquor are extremely complex, the fermentation liquor also comprises thalli, residual sugar, inorganic salt, protein, pigment, organic mixed acid and other impurities besides the product citric acid, the calcium salt extraction method is widely used by citric acid production enterprises due to mature technology and simple and convenient operation, but the calcium salt method has high labor intensity and low yield, the generated calcium sulfate waste residue seriously pollutes the environment, so that the novel extraction technology is selected to be an urgent problem, and the ion exchange method for citric acid extraction has the advantages of simple technology, easy operation, automatic operation and high yield, Low energy consumption and the like.
After citric acid is subjected to ion exchange, SO is mainly adsorbed on anion exchange resin4 2-，C1-In which SO4 2-As the main component, after the anion exchange resin is used for a period of time, the adsorbed impurities are close to saturation, and the anion exchange resin needs to be regenerated.
The existing anion exchange resin is regenerated and uses ammonia water for back flushing, so that only OH is on the anion exchange resin-The ammonia water can not be reused after the washing, so that the resources can not be reused, thereby wasting the resources.
Disclosure of Invention
The invention aims to: aims to solve the problem that only OH is on anion exchange resin because ammonia water is used for backflushing in the prior art-The method has the advantages that the method has activity again, but the ammonia water after washing can not be reused, so that resources can not be reused, and the resources are wasted.
In order to achieve the purpose, the invention provides the following technical scheme: a method for treating anion exchange resin by ammonia water comprises the steps of ammonia water, barium chloride and deionized water, wherein the ammonia water is a regenerant, the barium chloride is a precipitator, and the deionized water is a cleaning agent, and the treatment method comprises the following steps:
the method comprises the following steps: introducing deionized water to the bottom of the ion exchange column filled with the anion exchange resin to carry out backwashing on the ion exchange resin, wherein the backwashing time is 30-40 minutes;
step two: then, ammonia water with the mass fraction of 25-40% is used in an amount which is 1.5-3.5 times of the volume of the ion exchange resin, and the anion exchange resin treated in the first step is regenerated in a countercurrent mode at the regeneration flow rate of 4-10m/h for 30-40 min;
step three: introducing deionized water into the anion exchange resin treated in the second step from top to bottom for forward washing, and stopping washing until the pH value of discharged water reaches 8.0-9.0 to obtain regenerated anion exchange resin;
step four: adding barium hydroxide into the water obtained after the third washing step, and fully stirring, mixing and standing the water for 30-40 min;
step five: the BaSO obtained in the fourth step4Insoluble in water to generate precipitate, removing impurities, and oven drying to obtain BaSO4Powdering, and recycling the obtained ammonia water;
step six: the anion exchange resin and BaSO obtained by the steps4Collecting and storing the powder.
Preferably, when the ammonia water is used for regenerating the resin in the step two, a compaction layer is arranged on the top layer of the ion exchange resin, the compaction layer is composed of inert resin white balls, and the height of the compaction layer is 150-200 mm.
Preferably, in step four:
the chemical reaction formula is as follows: ba (OH)2+(NH4)2SO4＝BaSO4(white precipitate) +2NH3(gas) +2H2O；
Ion(s)The reaction formula is as follows: 2NH4+SO4 2-+Ba2++2OH-＝BaSO4(white precipitate) +2NH3(gas) +2H2O。
Preferably, in the step five:
the chemical reaction formula is as follows: NH (NH)3+2H2O＝NH3·H2O。
Compared with the prior art, the invention has the beneficial effects that: in the process of regenerating ion exchange resin, barium hydroxide is added to fully stir and stand with the water solution for washing the regenerated ion exchange resin to obtain barium sulfate precipitate and ammonia water, and the barium sulfate can be applied to the field of medical treatment; the ammonia water can be repeatedly used, the production cost is greatly reduced, and the resource is recycled.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
A method for treating anion exchange resin by ammonia water comprises the following steps of:
the method comprises the following steps: introducing deionized water to the bottom of the ion exchange column filled with the anion exchange resin for backwashing, wherein the backwashing time is 30 minutes;
step two: then, ammonia water with the mass fraction of 25% is used in an amount which is 1.5 times of the volume of the ion exchange resin, and the resin is regenerated for 30min by adopting a countercurrent mode and passing through the anion exchange resin treated in the first step at a regeneration flow rate of 5 m/h;
step three: introducing deionized water into the anion exchange resin treated in the second step from top to bottom for forward washing, and stopping washing until the pH value of discharged water reaches 8.0 to obtain regenerated anion exchange resin;
step four: adding barium hydroxide into the water obtained after the third washing step, and fully stirring, mixing and standing the water for 30 min;
step five: the BaSO obtained in the fourth step4Insoluble in water to generate precipitate, removing impurities, and oven drying to obtain BaSO4Powdering, and recycling the obtained ammonia water;
step six: the anion exchange resin and BaSO obtained by the steps4Collecting and storing the powder.
Example two
A method for treating anion exchange resin by ammonia water comprises the following steps of:
the method comprises the following steps: introducing deionized water to the bottom of the ion exchange column filled with the anion exchange resin to carry out backwashing on the ion exchange resin, wherein the backwashing time is 35 minutes;
step two: then, ammonia water with the mass fraction of 30% is used in an amount which is 2 times of the volume of the ion exchange resin, the resin is regenerated by adopting a countercurrent mode and passing through the anion exchange resin treated in the first step at a regeneration flow rate of 7.5m/h, and the regeneration is carried out for 35 min;
step three: introducing deionized water into the anion exchange resin treated in the second step from top to bottom for forward washing, and stopping washing until the pH value of discharged water reaches 8.5 to obtain regenerated anion exchange resin;
step four: adding barium hydroxide into the water obtained after the third washing step, and fully stirring, mixing and standing the water for 35 min;
step five: the BaSO obtained in the fourth step4Insoluble in water to generate precipitate, removing impurities, and oven drying to obtain BaSO4Powdering, and recycling the obtained ammonia water;
step six: the anion exchange resin and BaSO obtained by the steps4Collecting and storing the powder.
EXAMPLE III
A method for treating anion exchange resin by ammonia water comprises the following steps of:
the method comprises the following steps: introducing deionized water to the bottom of the ion exchange column filled with the anion exchange resin for backwashing, wherein the backwashing time is 40 minutes;
step two: then, ammonia water with the mass fraction of 40% is used in an amount which is 3.5 times of the volume of the ion exchange resin, the resin is regenerated by adopting a countercurrent mode and passing through the anion exchange resin treated in the first step at a regeneration flow rate of 10m/h for 40 min;
step three: introducing deionized water into the anion exchange resin treated in the second step from top to bottom for forward washing, and stopping washing until the pH value of discharged water reaches 9.0 to obtain regenerated anion exchange resin;
step four: adding barium hydroxide into the water obtained after the third washing step, and fully stirring, mixing and standing the water for 40 min;
step five: the BaSO obtained in the fourth step4Insoluble in water to generate precipitate, removing impurities, and oven drying to obtain BaSO4Powdering, and recycling the obtained ammonia water;
step six: the anion exchange resin and BaSO obtained by the steps4Collecting and storing the powder.
Through the first embodiment, the second embodiment and the third embodiment, barium sulfate precipitate can be obtained under different data, and ammonia water are reused, and corresponding ammonia water and barium hydroxide are added according to the quantity of the anion resin to be regenerated, so that the best effect is achieved.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (4)
1. A method for treating anion exchange resin by ammonia water comprises the steps of ammonia water, barium chloride and deionized water, and is characterized in that: the ammonia water is a regenerant, the barium chloride is a precipitator, and the deionized water is a cleaning agent, and the treatment method comprises the following steps:
the method comprises the following steps: introducing deionized water to the bottom of the ion exchange column filled with the anion exchange resin to carry out backwashing on the ion exchange resin, wherein the backwashing time is 30-40 minutes;
step two: then, ammonia water with the mass fraction of 25-40% is used in an amount which is 1.5-3.5 times of the volume of the ion exchange resin, and the anion exchange resin treated in the first step is regenerated in a countercurrent mode at the regeneration flow rate of 4-10m/h for 30-40 min;
step three: introducing deionized water into the anion exchange resin treated in the second step from top to bottom for forward washing, and stopping washing until the pH value of discharged water reaches 8.0-9.0 to obtain regenerated anion exchange resin;
step four: adding barium hydroxide into the water obtained after the third washing step, and fully stirring, mixing and standing the water for 30-40 min;
step five: the BaSO obtained in the fourth step4Insoluble in water to generate precipitate, removing impurities, and oven drying to obtain BaSO4Powdering, and recycling the obtained ammonia water;
step six: the anion exchange resin and BaSO obtained by the steps4Collecting and storing the powder.
2. A process for the treatment of anion exchange resins with aqueous ammonia according to claim 1, characterized in that: and when the ammonia water is used for regenerating the resin in the second step, a compaction layer is arranged on the top layer of the ion exchange resin, the compaction layer is composed of inert resin white balls, and the height of the compaction layer is 150-200 mm.
3. A process for the treatment of anion exchange resins with aqueous ammonia according to claim 1, characterized in that: in the fourth step:
the chemical reaction formula is as follows: ba (OH)2+(NH4)2SO4＝BaSO4(white precipitate) +2NH3(gas) +2H2O；
The ion reaction formula: 2NH4+SO4 2-+Ba2++2OH-＝BaSO4(white precipitate) +2NH3(gas) +2H2O。
4. A process for the treatment of anion exchange resins with aqueous ammonia according to claim 1, characterized in that: in the fifth step:
the chemical reaction formula is as follows: NH (NH)3+2H2O＝NH3·H2O。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011574897.0A CN112808323A (en) | 2020-12-28 | 2020-12-28 | Method for treating anion exchange resin by ammonia water |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011574897.0A CN112808323A (en) | 2020-12-28 | 2020-12-28 | Method for treating anion exchange resin by ammonia water |
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| Publication Number | Publication Date |
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| CN112808323A true CN112808323A (en) | 2021-05-18 |
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| CN202011574897.0A Pending CN112808323A (en) | 2020-12-28 | 2020-12-28 | Method for treating anion exchange resin by ammonia water |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1464007A (en) * | 1974-04-23 | 1977-02-09 | Dynamit Nobel Ag | Regeneration of ion exchange resins |
| US20050182147A1 (en) * | 2004-02-17 | 2005-08-18 | Institute Of Nuclear Energy Research Atomic Energy Council | Method for processing spent ion-exchange resins |
| US20070114178A1 (en) * | 2005-11-23 | 2007-05-24 | Coppola Edward N | Water treatment process for perchlorate, nitrate, chromate, arsenate and other oxyanions for using weak-base anion exchange resins |
| CN101774644A (en) * | 2009-09-28 | 2010-07-14 | 贵州红星发展股份有限公司 | Method for preparing Mn(OH)2 by circularly using ammonia water |
| CN102260167A (en) * | 2011-08-04 | 2011-11-30 | 中粮生物化学（安徽）股份有限公司 | Treatment method of citric acid contained solution |
| CN103638994A (en) * | 2013-12-03 | 2014-03-19 | 日照鲁信金禾生化有限公司 | Method for treating anion exchange resin by using ammonia water |
-
2020
- 2020-12-28 CN CN202011574897.0A patent/CN112808323A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1464007A (en) * | 1974-04-23 | 1977-02-09 | Dynamit Nobel Ag | Regeneration of ion exchange resins |
| US20050182147A1 (en) * | 2004-02-17 | 2005-08-18 | Institute Of Nuclear Energy Research Atomic Energy Council | Method for processing spent ion-exchange resins |
| US20070114178A1 (en) * | 2005-11-23 | 2007-05-24 | Coppola Edward N | Water treatment process for perchlorate, nitrate, chromate, arsenate and other oxyanions for using weak-base anion exchange resins |
| CN101774644A (en) * | 2009-09-28 | 2010-07-14 | 贵州红星发展股份有限公司 | Method for preparing Mn(OH)2 by circularly using ammonia water |
| CN102260167A (en) * | 2011-08-04 | 2011-11-30 | 中粮生物化学（安徽）股份有限公司 | Treatment method of citric acid contained solution |
| CN103638994A (en) * | 2013-12-03 | 2014-03-19 | 日照鲁信金禾生化有限公司 | Method for treating anion exchange resin by using ammonia water |
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