CN101817560A - Methods for removing calcium and magnesium alkaline-earth metal ions contained in chromate solution by adopting ion exchange resin - Google Patents
Methods for removing calcium and magnesium alkaline-earth metal ions contained in chromate solution by adopting ion exchange resin Download PDFInfo
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- CN101817560A CN101817560A CN201010142709A CN201010142709A CN101817560A CN 101817560 A CN101817560 A CN 101817560A CN 201010142709 A CN201010142709 A CN 201010142709A CN 201010142709 A CN201010142709 A CN 201010142709A CN 101817560 A CN101817560 A CN 101817560A
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- ion exchange
- exchange resin
- resin
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- chromate solution
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Abstract
The invention relates to a method for removing calcium and magnesium alkaline-earth metal ions contained in a chromate solution by adopting ion exchange resin, belonging to the technical field of refining of the chromate solution. A process course comprises the following steps of: adding a chemical refined preparation to remove a large majority of impurities; filtering suspended matters contained in the suspended matter by using a filter to obtain a chromate solution with suspended matter content less than 1 mg/L; dynamically contacting the obtained chromate solution with the ion exchange resin to carry out ion exchange; and diluting or concentrating the obtained chromate solution to prepare a feed solution suitable for electrolysis. The invention has the advantages that the chromate solution containing obviously reduced calcium and magnesium can be obtained and is very suitable for being used as the feed solution of chromate synthesized into dichromate till chromic anhydride through electrocatalysis; and the ion exchange resin saturated by adsorption can be repeatedly used by being washed, regenerated and transformed; and in addition, the method has the advantages of moderate process condition, easy operation, little pollution, low cost and easy resin regeneration, and can realize the continuous large-scale production.
Description
Technical field
The invention belongs to the purification techniques field of chromatedsolution, be specifically related to a kind of method that adopts ion exchange resin to remove calcium, magnesium alkaline-earth metal ions in the chromatedsolution, the solution after making with extra care is applicable to as the stock liquid of the synthetic dichromate of chromic salt electrocatalysis until chromic trioxide.
Background technology
Chromic trioxide is called for short chromic anhydride, and molecular formula is: CrO
3, be a kind of important chromaking chemical product, be strong oxidizer, very easily deliquescence is soluble in water, and corrodibility is extremely strong, and is poisonous.In the chromic salts product, chromic trioxide accounts for 60% of ultimate production, is mainly used in preparation water soluble timber sanitas chromium cupric arsenate, secondly is to be used for Metal Finishing, controlling catalyst, chromium sesquioxide and magneticsubstance chromium dioxide and to be used as oxygenant, mordant etc.
In traditional processing technology, Na
2Cr
2O
7-H
2SO
4Technology such as batch melting method, outer hot continuous processing, self-heating continuous processing, wet method, generation contains chromium Na in a large number
2SO
4And NaHSO
4Byproduct, and high toxicity chromium slag, environmental pollution is extremely serious.Ionic membrane electrocatalysis synthesis of chromic anhydride new cleanproduction process, it is the important component part of process engineering institute of Chinese Academy of Sciences chromic salts cleaner production integrated technology, this flow process does not consume sodium hydroxide/potassium in theory, except that producing the major product chromic trioxide, byproduct sodium hydroxide/potassium, oxygen, hydrogen are the raw material of other operation of novel process, can realize full-range refuse zero release.Sodium chromate/potassium is the important source material of ionic membrane method electrocatalysis synthesis of chromic anhydride, and ionic membrane method electrocatalysis synthesis of chromic anhydride technology requires high to calcium, the magnesium alkaline earth polyvalent metal ion foreign matter content that enters in the chromic salt in the anode electrolytic tank, otherwise in electrocatalysis is synthetic, polyvalent cation in the anolyte can combine with the negatively charged ion from the catholyte backmigration in the process of catholyte migration, form precipitation of hydroxide, the plug ion exchange membrane, cause bath voltage to rise, power consumption increases, and current efficiency descends.At present, Sodium chromate/potassium solution is removed the method for micro-calcium, magnesium addition, adopts chemical precipitation method to handle more, produces big solid waste pollution, operates miscellaneously, and labour intensity is big, and is difficult to make highly purified product.In addition, also have methods such as membrane sepn, electrodialysis, all seldom use because the production cost height maybe can not obtain closing the product of clothes requirement.Ion exchange method is to utilize the cation exchange groups of ion exchange resin, and absorption, exchange, chelated metal ions adopt eluent that the ion that absorption, exchange, chelating get on is eluted then, thus the purpose that reaches separation, purifies.This method has easy handling, pollute few, can access purer product, be widely used in carrying uranium in the preparation, nuclear industry of processing, electronic industry high purity water, the ultra-high purity water of softening, the trade effluent of boiler feed water and radioactive wastewater is handled, be applicable to industries such as extractions, separation, concentrated, purification.Japan's publication (flat 2-107526) has been introduced a kind of process for purification of chromium acid sodium solution, but it can only drop to 0.4ppm with calcium, magnesium at most.
Summary of the invention
The purpose of this invention is to provide a kind of method that adopts ion exchange resin to remove calcium, magnesium alkaline-earth metal ions in the chromatedsolution, chromic salt after refining obviously reduces wherein calcium, magnesium addition content, can be used for as the raw material of the synthetic dichromate of electrocatalysis until chromic trioxide; Realized that processing condition are not harsh, simple to operate, polluted and lack that cost is low, resin regeneration is easy, can realize serialization scale operation.
The present invention exchanges calcium, the magnesium of removing in the chromatedsolution with the ion exchange resin that has phosphoramidic acid or imido oxalic acid functional group.Technological process is:
A. the K that adds excessive 0.2-0.82g/L earlier
2CO
3Or Na
2CO
3, add excessive 0.004-0.016g/L KOH or NaOH finishing agent again and remove wherein most of impurity;
B. with strainer the suspended substance in the chromic salt is filtered, obtain the chromatedsolution of suspension content less than 1mg/L;
C. the gained chromatedsolution is dynamically contacted with ion exchange resin and carry out ion-exchange;
D. the chromatedsolution that is obtained by step c is applicable to electrolytic stock liquid through dilution or concentrated making.
Chromic salt of the present invention is Sodium chromate or potassiumchromate.
Described ion exchange resin be have imido oxalic acid or phosphoramidic acid chelation group crosslinked granules of polystyrene polymkeric substance.
Described ion-exchange is to carry out in ion exchange column, the used ion exchange column intermediate ion exchange resin loading height and the ratio of column diameter are between 10: 1 to 25: 1, temperature is controlled at 20 ℃-80 ℃, and the pH value is controlled at 8.5-11.5, and the dynamic method flow velocity is 1-8ml/min; Alkalimetal ion in calcium in the solution, magnesium ion and the ion exchange resin exchanges, thereby reaches the purpose that reduces calcium, magnesium ion concentration in the solution.
Described chromium acid sodium solution concentration is 100-600g/L, and potassium chromate solution concentration is 100-450g/L.
The mean pore size of described strainer is between the 0.1-0.4 micron.
Described ion exchange resin can be reused, the ion exchange resin elder generation water that the steps include: to adsorb after saturated is washed residual solution and impurity off, use the hydrochloric acid drip washing of 3-5% again, to near neutral, with the alkaline solution of 3-6% ion exchange resin is made the transition then is K to resin after the drip washing with pure water washing
+Type or Na
+Type, transition, back ion exchange resin washed with ultrapure water, until approaching neutral.
Resin absorption, regeneration principle are:
(1) adsorption process of resin reaction
R (N
+)
2+ M
2+→ RM
2++ 2N
+(M
2+=Ca
2+Or Mg
2+, N
+=K
+Or Na
+)
(2) regeneration of resin process reaction
RM
2++2H
+→RH
++M
2+
Reaction transition of resin
RH
++N
+→RN
++H
+
The saturated Ca of resin absorption
2+Or Mg
2+After, through washing, regeneration, transition, repeated use promptly capable of circulation.
The invention has the advantages that, can obtain the obviously chromatedsolution of decline of calcium, magnesium, this solution is highly suitable for as the stock liquid of the synthetic dichromate of chromic salt electrocatalysis until chromic trioxide.Adsorb the ion exchange resin after saturated, through washing, regeneration, transition, resin can be reused.This method processing condition gentleness, simple to operate, pollute and lack, cost is low, and resin regeneration is easy, can realize serialization scale operation.
Embodiment
Embodiment 1:
The DA460 vinylbenzene phosphoramidic acid acid ion exchange resin that adopts the big chemical industry group in east, Shandong to produce is removed calcium, magnesium from potassium chromate solution.Its technological process is:
A. first K with excessive 0.3g/L
2CO
3With excessive 0.01g/LKOH solution most of polyvalent metal ion in the 250g/L potassium chromate solution is removed, again potassium chromate solution is filtered in 0.4 micron filter;
B. the pH value of potassium chromate solution does not adjust;
C. the speed with 5ml/min is 35cm by the post height from the bottom with potassium chromate solution, and diameter is the ion exchange column that 1.82cm is equipped with DA460 ion exchange resin;
D. ion exchange column has the water cycle heating jacket outward, and making temperature is 65 ℃.Calcium in the potassium chromate solution, magnesium ion are reduced to 0.089mg/L and 0.073mg/L respectively from initial 6mg/L and 3mg/L.Resin purified rinse water after the adsorption penetration is to remove folder stays in the resin impurity and bubble etc.Carry out counter-current regeneration with 4% hydrochloric acid soln then, after regeneration finishes, be washed with water to neutrality, use again 5% potassium hydroxide solution with ion exchange resin conversion to K
+Type washes with water to neutrality, and resin is repeated use capable of circulation.
Embodiment 2:
Adopt German Bayer AG to produce TP207 vinylbenzene iminodiethanoic acid ion exchange resin, from chromium acid sodium solution, remove calcium, magnesium.Its technological process is:
A. use earlier excessive 0.2g/LNa
2CO
3With excessive 0.008g/LNaOH solution most of polyvalent metal ion in the 200g/L chromium acid sodium solution is removed, again chromium acid sodium solution is filtered in 0.2 micron filter;
B. adjusting the pH value is 9.5;
C. the speed with 2ml/min is 20cm by the post height from the bottom with chromium acid sodium solution, and diameter is the ion exchange column that 1.68cm is equipped with TP207 ion exchange resin;
D. ion exchange column has the water cycle heating jacket outward, and making temperature is 50 ℃.Calcium in the chromium acid sodium solution, magnesium ion are reduced to 0.112mg/L and 0.109mg/L respectively from initial 9mg/L and 4mg/L.Resin purified rinse water after the adsorption penetration is to remove folder stays in the resin impurity and bubble etc.Carry out co-current regeneration with 3% hydrochloric acid soln then, after regeneration finishes, be washed with water to neutrality, use again 5% sodium hydroxide solution with ion exchange resin conversion to Na
+Type washes with water to neutrality, and resin is repeated use capable of circulation.
Embodiment 3:
The Amberlite IRC 748 vinylbenzene iminodiethanoic acid ion exchange resin that adopt U.S. sieve Haars Co., Ltd to produce remove calcium-magnesium removing from potassium chromate solution.Its technological process is:
A. use earlier excessive 0.5g/LK
2CO
3With excessive 0.012g/LKOH solution most of polyvalent metal ion in the 450g/L potassium chromate solution is removed, again potassium chromate solution is filtered in 0.4 micron filter;
B. the pH value of potassium chromate solution does not adjust;
C. the speed with 1ml/min is 25cm by the post height from the top with potassium chromate solution, and diameter is the ion exchange column that 1.68cm is equipped with 748 ion exchange resin;
D. ion exchange column has the water cycle heating jacket outward, and making temperature is 50 ℃.Calcium in the potassium chromate solution, magnesium ion are reduced to 0.092mg/L and 0.065mg/L respectively from initial 10mg/L and 7mg/L.Resin purified rinse water after the adsorption penetration is to remove folder stays in the resin impurity and bubble etc.Carry out counter-current regeneration with 4% hydrochloric acid soln then, after regeneration finishes, be washed with water to neutrality, use again 5% potassium hydroxide solution with ion exchange resin conversion to K
+Type washes with water to neutrality, and resin is repeated use capable of circulation.
Embodiment 4:
The Amberlite IRC 747 vinylbenzene phosphoramidic acid ion exchange resin that adopt U.S. sieve Haars Co., Ltd to produce are removed calcium, magnesium from chromium acid sodium solution.Its technological process is:
A. use earlier excessive 0.6g/LNa
2CO
3With excessive 0.009g/LNaOH solution most of polyvalent metal ion in the 550g/L chromium acid sodium solution is removed, again chromium acid sodium solution is filtered in 0.2 micron filter;
B. the pH with chromium acid sodium solution is adjusted into 9.5;
C. the speed with 3ml/min is 30cm by the post height from the top with chromium acid sodium solution, and diameter is the ion exchange column that 1.82cm is equipped with Amberlite IRC 747 ion exchange resin;
D. ion exchange column has the water cycle heating jacket outward, and making temperature is 55 ℃.Calcium in the chromium acid sodium solution, magnesium ion are reduced to 0.062mg/L and 0.051mg/L respectively from initial 5mg/L and 3mg/L.Resin purified rinse water after the adsorption penetration is to remove folder stays in the resin impurity and bubble etc.Carry out co-current regeneration with 4% hydrochloric acid soln then, after regeneration finishes, be washed with water to neutrality, use again 6% sodium hydroxide solution with ion exchange resin conversion to Na
+Type washes with water to neutrality, and resin is repeated use capable of circulation.
Claims (6)
1. method that adopts ion exchange resin to remove calcium, magnesium alkaline-earth metal ions in the chromatedsolution is characterized in that technological process is:
A. the K that adds excessive 0.2-0.82g/L earlier
2CO
3Or Na
2CO
3, add excessive 0.004-0.016g/LKOH or NaOH finishing agent again and remove wherein most of impurity;
B. with strainer the suspended substance in the chromic salt is filtered, obtain the chromatedsolution of suspension content less than 1mg/L;
C. the gained chromatedsolution is dynamically contacted with ion exchange resin and carry out ion-exchange;
D. the chromatedsolution that is obtained by step c is applicable to electrolytic stock liquid through dilution or concentrated making.
2. according to the method for claim 1, it is characterized in that described chromic salt is Sodium chromate or potassiumchromate.
3. method according to claim 1 is characterized in that, described ion exchange resin be have imido oxalic acid or phosphoramidic acid chelation group crosslinked granules of polystyrene polymkeric substance.
4. according to claim 1 or 4 described methods, it is characterized in that, described ion-exchange is to carry out in ion exchange column, the used ion exchange column intermediate ion exchange resin loading height and the ratio of column diameter are between 10: 1 to 25: 1, temperature is controlled at 20 ℃-80 ℃, the pH value is controlled at 8.5-11.5, and the dynamic method flow velocity is 1-8ml/min.
5. method according to claim 1 is characterized in that, described chromium acid sodium solution concentration is 100-600g/L, and potassium chromate solution concentration is 100-450g/L; The mean pore size of described strainer is the 0.1-0.4 micron.
6. method according to claim 1, it is characterized in that, described ion exchange resin is reused, the ion exchange resin elder generation water that the steps include: to adsorb after saturated is washed residual solution and impurity off, use the hydrochloric acid drip washing of 3-5% again, to near neutral, with the alkaline solution of 3-6% ion exchange resin is made the transition then is K to resin after the drip washing with pure water washing
+Type or Na
+Type, transition, back ion exchange resin washed with ultrapure water, until approaching neutral; The adsorption process reaction of resin: R (N
+)
2+ M
2+→ RM
2++ 2N
+, regeneration of resin process reaction: RM
2++ 2H
+→ RH
++ M
2+, reaction transition of resin: RH
++ N
+→ RN
++ H
+
The saturated Ca of resin absorption
2+Or Mg
2+After, through washing, regeneration, transition, circulation is reused.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010142709A CN101817560A (en) | 2010-04-07 | 2010-04-07 | Methods for removing calcium and magnesium alkaline-earth metal ions contained in chromate solution by adopting ion exchange resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010142709A CN101817560A (en) | 2010-04-07 | 2010-04-07 | Methods for removing calcium and magnesium alkaline-earth metal ions contained in chromate solution by adopting ion exchange resin |
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|---|---|
| CN101817560A true CN101817560A (en) | 2010-09-01 |
Family
ID=42652864
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010142709A Pending CN101817560A (en) | 2010-04-07 | 2010-04-07 | Methods for removing calcium and magnesium alkaline-earth metal ions contained in chromate solution by adopting ion exchange resin |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815765A (en) * | 2012-08-30 | 2012-12-12 | 中国石油天然气股份有限公司 | Deep softening method of thick oil sewage |
| CN107226485A (en) * | 2017-07-03 | 2017-10-03 | 信丰华锐钨钼新材料有限公司 | A kind of method of deep removal calcium, magnesium from sodium molybdate solution |
| CN108975361A (en) * | 2018-10-09 | 2018-12-11 | 广东海洋大学 | A kind of magnesium hydroxide soil conditioner prepared using magnesium elements in seawater |
| CN110980876A (en) * | 2019-11-21 | 2020-04-10 | 武汉百富环保工程有限公司 | Treatment process for recovering copper and recycling chromium from passivation solution |
| CN115010292A (en) * | 2022-05-30 | 2022-09-06 | 金川集团镍盐有限公司 | Method for removing Ca ions and Mg ions in nickel-containing wastewater |
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2010
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Non-Patent Citations (6)
| Title |
|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815765A (en) * | 2012-08-30 | 2012-12-12 | 中国石油天然气股份有限公司 | Deep softening method of thick oil sewage |
| CN107226485A (en) * | 2017-07-03 | 2017-10-03 | 信丰华锐钨钼新材料有限公司 | A kind of method of deep removal calcium, magnesium from sodium molybdate solution |
| CN108975361A (en) * | 2018-10-09 | 2018-12-11 | 广东海洋大学 | A kind of magnesium hydroxide soil conditioner prepared using magnesium elements in seawater |
| CN110980876A (en) * | 2019-11-21 | 2020-04-10 | 武汉百富环保工程有限公司 | Treatment process for recovering copper and recycling chromium from passivation solution |
| CN115010292A (en) * | 2022-05-30 | 2022-09-06 | 金川集团镍盐有限公司 | Method for removing Ca ions and Mg ions in nickel-containing wastewater |
| CN115010292B (en) * | 2022-05-30 | 2023-10-03 | 金川集团镍盐有限公司 | Method for removing Ca ions and Mg ions in nickel-containing wastewater |
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Application publication date: 20100901 |