CN102730722A - Method for preparing refined strong brine by removing potassium from strong brine - Google Patents

Method for preparing refined strong brine by removing potassium from strong brine Download PDF

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CN102730722A
CN102730722A CN2012102455341A CN201210245534A CN102730722A CN 102730722 A CN102730722 A CN 102730722A CN 2012102455341 A CN2012102455341 A CN 2012102455341A CN 201210245534 A CN201210245534 A CN 201210245534A CN 102730722 A CN102730722 A CN 102730722A
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strong brine
potassium
ion exchange
exchange column
raw material
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CN102730722B (en
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袁俊生
纪志永
郭小甫
谢英惠
刘杰
王军
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Hebei eight dimension Chemical Co., Ltd.
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Hebei University of Technology
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Abstract

The invention provides a method for preparing refined strong brine by removing potassium from strong brine, and relates to a method for removing potassium from strong brine. The method comprises the following steps of: under the temperature of 15-40DEG C, introducing raw material strong brine into an ion exchange column filled with modified zeolite to carry out an adsorbing reaction, adsorbing the raw material strong brine by an analogue moving bed technology till exchange reaction between the potassium ions in the raw material strong brine and the sodium ions on the modified zeolite is completed, and adsorbing to obtain the refined strong brine of which the K<+> content is 0.10g/L-0.39g/L; and eluting potassium ions in the ion exchange column after adsorption in the first step by taking saturated sodium chloride solution as eluant under the temperature of 25-95DEG C, so that the potassium-rich solution of which the potassium ion concentration is 10.23g/L-12.67g/L can be obtained, and the ion exchange column can be recycled after being eluted by the saturated sodium chloride solution. According to the method provided by the invention, the potassium ions in the electrically-dialysed strong brine can be effectively removed, and the qualified brine which meets the requirement of the chlor-alkali industry can be prepared.

Description

From strong brine, remove the method for the refining strong brine of potassium preparation
Technical field
Technical scheme of the present invention relates to removes potassium from salt solution, specifically from strong brine, remove the method for the refining strong brine of potassium preparation.
Background technology
Refining strong brine mainly contains two big purposes, and the one, be used for salt manufacturing, the 2nd, be used for chlor-alkali industry.Because the main source of salt is a seawater; Follow the aggravation of coastland land used pressure; Batch production salt manufacturing will finally replace tradition and evaporate brine; Particularly following the development of extensive sea water desaltination industry, is raw material with seawater or concentrated seawater, is that the batch production salt manufacturing pattern of representative will be adopted gradually with electrodialysis system liquid salt.The strong brine that obtains after the electrodialysis generally contains a spot of K +, Ca 2+, Mg 2+And SO 4 2-, Ca in the salt solution 2+, Mg 2+And SO 4 2-Removal come into one's own always, the removal method is comparatively ripe.For example, CN1107121A discloses a kind of " utilizing bittern to prepare the method for refined brine ", mainly is to utilize precipitin reaction to remove the Ca in bittern and the salt solution 2+, Mg 2+, SO 4 2-CN1019095B discloses " a kind of method that purifies sodium chloride brine and bittern ", mainly is the SO that removes in salt solution and the bittern 4 2-And Ca 2+CN1147429C discloses a kind of method of refined brine, mainly is the calcium magnesium of removing in the salt solution.In the process for refining of the strong brine that behind existing electroosmose process, obtains, to K +Removal also do not have what effective means, and K +Existence directly influence the purity of quality, the especially caustic soda of chlor-alkali industry product.Therefore, the strong brine that obtains after the refining electrodialysis is particularly removed K wherein +, be the chlor-alkali industry active demand to make the qualified salt solution that satisfies the chlor-alkali industry requirement.At present, do not see as yet the relevant strong brine that behind electroosmose process, obtains and remove K +Make the bibliographical information of refining strong brine.
Summary of the invention
Technical problem to be solved by this invention is: the method for from strong brine, removing the refining strong brine of potassium preparation is provided; It is a kind of method of removing the refining strong brine of potassium preparation with modified zeolite; Can remove the potassium ion in the strong brine that obtains after the electrodialysis effectively, to make the qualified salt solution that satisfies the chlor-alkali industry requirement.
The present invention solves this technical problem the technical scheme that is adopted: from strong brine, removing the method for the refining strong brine of potassium preparation, is a kind of with the method for modified zeolite except that the refining strong brine of potassium preparation, and concrete steps are:
The first step, the absorption of carrying out the raw material strong brine with the ion exchange column that loads modified zeolite removes potassium, makes refining strong brine
Under 15~40 ℃; Carry out absorption reaction in the ion exchange column with raw material strong brine feeding filling modified zeolite; Complete with simulated moving bed technology to potassium ion and the sodium ion generation permutoid reaction on the modified zeolite that the raw material strong brine is adsorbed in the raw material strong brine, obtain K after the suction +Content is the refining strong brine of 0.10g/L~0.39g/L;
In second step, the potassium ion in the ion exchange column after inhaling is carried out wash-out
Under 25 ℃~95 ℃ temperature with saturated nacl aqueous solution as eluent to the first step in absorption after ion exchange column in potassium ion carry out wash-out; Obtain containing the rich potassium solution that potassium concentration is 10.23g/L~12.67g/L, this ion exchange column is through recycle after the wash-out of saturated nacl aqueous solution.
The above-mentioned method of from strong brine, removing the refining strong brine of potassium preparation, said raw material strong brine is the strong brine that obtains after the electrodialysis.
The above-mentioned method of from strong brine, removing the refining strong brine of potassium preparation; The ion exchange column of said filling modified zeolite is divided into by 6~12 single ion exchange column that 2~4 operating units form; Every single ion exchange column is by being 36mm at diameter and highly be to load modified zeolite 800g in the cylinder of 1000mm to constitute, and 3 ion exchange columns are set at an operating unit.
The above-mentioned method of from strong brine, removing the refining strong brine of potassium preparation; The concrete technology of described simulated moving bed technology is; Packed height in the control ion exchange column is 6m~12m; Every 3m is an operating unit, and each operating unit feeds strong brine 3L~21L, and the absorption flow velocity of raw material strong brine is that the void tower flow rate control is at 7m/h~12m/h.
The above-mentioned method of from strong brine, removing the refining strong brine of potassium preparation; The strong brine that obtains after the used raw material electrodialysis, modified zeolite, ion exchange column cylinder and saturated nacl aqueous solution all obtain through known approach easily, and described technology is that those skilled in the art knows.
The invention has the beneficial effects as follows: compared with prior art, the present invention removes the method for the refining strong brine of potassium preparation from strong brine marked improvement is:
(1) removes potassium in the strong brine that obtains after the electrodialysis effectively, K in the refining strong brine that obtains after the suction +Content is 0.10g/L~0.39g/L, must make with extra care strong brine after the suction and promptly can be used for chlor-alkali industry, and being applied to the caustic soda industry can effectively improve the quality of products, and makes high-purity caustic soda.
(2), save its traditional change salt operation and reach demand fresh water simultaneously for chlor-alkali industry provides Yan Heshui.
(3) adopt simulated moving bed technology, make K in the refining strong brine that obtains after the suction +Content is low and stable, and the potassium ion decreasing ratio can reach more than 95% in the salt solution; The rich potassium solution composition that obtains is uniform and stable
(4) the inventive method raw material is easy to get, technology is simple, low cost and efficient.
Embodiment
Embodiment 1
The first step, the absorption of carrying out the raw material strong brine with the ion exchange column that loads modified zeolite removes potassium
Under 25 ℃; Carry out absorption reaction in the ion exchange column with the strong brine feeding filling modified zeolite that obtains after the raw material electrodialysis; The ion exchange column of this filling modified zeolite is to be divided into 3 operating units by 9 single ion exchange column to form; Every single ion exchange column is by being 36mm at diameter and highly be to load modified zeolite 800g in the cylinder of 1000mm to constitute, and 3 ion exchange columns are set at an operating unit.Complete with simulated moving bed technology to potassium ion and the sodium ion generation permutoid reaction on the modified zeolite that the raw material strong brine is adsorbed in the raw material strong brine; Concrete technology is: the packed height in the control ion exchange column is 9m; Every 3m is an operating unit; Each operating unit feeds strong brine 3L, the absorption flow velocity of raw material strong brine be the void tower flow rate control at 7m/h, obtain K after the suction +Content is the refining strong brine of 0.39g/L, and the composition of strong brine is seen table 1 before and after modified zeolite absorption;
In second step, the potassium ion in the ion exchange column after inhaling is carried out wash-out
Under 95 ℃ of temperature with saturated nacl aqueous solution as eluent to the first step in absorption after ion exchange column in potassium ion carry out wash-out; Obtain 1.8L and contain the rich potassium solution that potassium concentration is 12.67g/L, be recycled after the wash-out of this ion exchange column through saturated nacl aqueous solution.The composition of the rich potassium solution that obtains after taking off is thus seen table 2.
Among table 1. embodiment 1 before and after modified zeolite absorption the composition of strong brine
Figure BDA00001895745400031
Among table 2. embodiment 1 with the composition of the rich potassium solution that obtains behind the saturated nacl aqueous solution wash-out
Figure BDA00001895745400032
Embodiment 2
The first step, the absorption of carrying out the raw material strong brine with the ion exchange column that loads modified zeolite removes potassium
Under 15 ℃; Carry out absorption reaction in the ion exchange column with raw material strong brine feeding filling modified zeolite; The ion exchange column of this filling modified zeolite is divided into by 12 single ion exchange column that 4 operating units form; Every single ion exchange column is by being 36mm at diameter and highly be to load modified zeolite 800g in the cylinder of 1000mm to constitute, and 3 ion exchange columns are set at an operating unit.Complete with simulated moving bed technology to potassium ion and the sodium ion generation permutoid reaction on the modified zeolite that the raw material strong brine is adsorbed in the raw material strong brine; Concrete technology is: the packed height in the control ion exchange column is 12m; Every 3m is an operating unit; Each operating unit feeds strong brine 8L, the absorption flow velocity of raw material strong brine be the void tower flow rate control at 10m/h, obtain K after the suction +Content is the refining strong brine of 0.13g/L, and the composition of strong brine is seen table 3 before and after modified zeolite absorption;
In second step, the potassium ion in the ion exchange column after inhaling is carried out wash-out
Under 60 ℃ of temperature with saturated nacl aqueous solution as eluent to the first step in absorption after ion exchange column in potassium ion carry out wash-out; Obtain 2.5L and contain the rich potassium solution that potassium concentration is 11.45g/L, be recycled after the wash-out of this ion exchange column through saturated nacl aqueous solution.The composition of the rich potassium solution that obtains after taking off is thus seen table 4.
Among table 3. embodiment 2 before and after modified zeolite absorption the composition of strong brine
Among table 4. embodiment 2 with the composition of the rich potassium solution that obtains behind the saturated nacl aqueous solution wash-out
Figure BDA00001895745400041
Embodiment 3
The first step, the absorption of carrying out the raw material strong brine with the ion exchange column that loads modified zeolite removes potassium
Under 40 ℃; Carry out absorption reaction in the ion exchange column with raw material strong brine feeding filling modified zeolite; The ion exchange column of this filling modified zeolite is divided into by 6 single ion exchange column that 2 operating units form; Every single ion exchange column is by being 36mm at diameter and highly be to load modified zeolite 800g in the cylinder of 1000mm to constitute, and 3 ion exchange columns are set at an operating unit.Complete with simulated moving bed technology to potassium ion and the sodium ion generation permutoid reaction on the modified zeolite that the raw material strong brine is adsorbed in the raw material strong brine; Concrete technology is: the packed height in the control ion exchange column is 6m; Every 3m is an operating unit; Each operating unit feeds strong brine 21L, the absorption flow velocity of raw material strong brine be the void tower flow rate control at 12m/h, obtain K after the suction +Content is the refining strong brine of 0.10g/L, and the composition of strong brine is seen table 5 before and after modified zeolite absorption;
In second step, the potassium ion in the ion exchange column after inhaling is carried out wash-out
Under 25 ℃ of degree with saturated nacl aqueous solution as eluent to the first step in absorption after ion exchange column in potassium ion carry out wash-out; Obtain containing the rich potassium solution that potassium concentration is 10.23g/L, be recycled after the wash-out of this ion exchange column through saturated nacl aqueous solution.The composition of the rich potassium solution that obtains after taking off is thus seen table 6.
Among table 5. embodiment 3 before and after modified zeolite absorption the composition of strong brine
Figure BDA00001895745400042
Among table 6. embodiment 3 with the composition of the rich potassium solution that obtains behind the saturated nacl aqueous solution wash-out
Figure BDA00001895745400043
In the foregoing description, the strong brine that obtains after the used raw material electrodialysis, modified zeolite, ion exchange column cylinder and saturated nacl aqueous solution all obtain through known approach easily, and described technology is that those skilled in the art knows.

Claims (4)

1. from strong brine, remove the method for the refining strong brine of potassium preparation, it is characterized in that: be a kind of with the method for modified zeolite except that the refining strong brine of potassium preparation, concrete steps are:
The first step, the absorption of carrying out the raw material strong brine with the ion exchange column that loads modified zeolite removes potassium, makes refining strong brine
Under 15~40 ℃; Carry out absorption reaction in the ion exchange column with raw material strong brine feeding filling modified zeolite; Complete with simulated moving bed technology to potassium ion and the sodium ion generation permutoid reaction on the modified zeolite that the raw material strong brine is adsorbed in the raw material strong brine, obtain K after the suction +Content is the refining strong brine of 0.10g/L~0.39g/L;
In second step, the potassium ion in the ion exchange column after inhaling is carried out wash-out
Under 25 ℃~95 ℃ temperature with saturated nacl aqueous solution as eluent to the first step in absorption after ion exchange column in potassium ion carry out wash-out; Obtain containing the rich potassium solution that potassium concentration is 10.23g/L~12.67g/L, this ion exchange column is through recycle after the wash-out of saturated nacl aqueous solution.
2. according to the said method of from strong brine, removing the refining strong brine of potassium preparation of claim 1, it is characterized in that: said raw material strong brine is the strong brine that obtains after the electrodialysis.
3. according to the said method of from strong brine, removing the refining strong brine of potassium preparation of claim 1; It is characterized in that: the ion exchange column of said filling modified zeolite is divided into by 6~12 single ion exchange column that 2~4 operating units form; Every single ion exchange column is by being 36 mm at diameter and highly be to load modified zeolite 800g in the cylinder of 1000 mm to constitute, and 3 ion exchange columns are set at an operating unit.
4. according to the said method of from strong brine, removing the refining strong brine of potassium preparation of claim 1; It is characterized in that: the concrete technology of described simulated moving bed technology is; Packed height in the control ion exchange column is 6m~12m; Every 3m is an operating unit, and each operating unit feeds strong brine 3L~21L, and the absorption flow velocity of raw material strong brine is that the void tower flow rate control is at 7m/h~12m/h.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107285430A (en) * 2016-04-05 2017-10-24 亚太森博(山东)浆纸有限公司 A kind of salt dissolving pond, chlor-alkali salt water treating system and chlor-alkali saline treatment technique
CN108996521A (en) * 2018-08-07 2018-12-14 泉州师范学院 A kind of technique using the selective electrodialysis concentration high-purity purified salt of brine production
CN112723388A (en) * 2020-12-25 2021-04-30 卢广荣 Preparation method of medical potassium-free micro-sodium salt

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6066257A (en) * 1998-08-04 2000-05-23 Calgon Carbon Corporation Process for the removal and destruction of perchlorate and nitrate from aqueous streams
WO2005009578A2 (en) * 2003-07-16 2005-02-03 Amalgamated Research, Inc. Method for the recovery of acids from hydrometallurgy process solutions
CN1747771A (en) * 2003-02-04 2006-03-15 独立行政法人产业技术总合研究所 Method of reducing impurity content in aqueous salt solution
CN100999364A (en) * 2006-05-16 2007-07-18 葛文宇 Comprehensive utilization high advantage zero discharge seawater desalination production technology
CN101850991A (en) * 2010-01-14 2010-10-06 河北工业大学 Method for preparing potassium chloride from seawater

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6066257A (en) * 1998-08-04 2000-05-23 Calgon Carbon Corporation Process for the removal and destruction of perchlorate and nitrate from aqueous streams
CN1747771A (en) * 2003-02-04 2006-03-15 独立行政法人产业技术总合研究所 Method of reducing impurity content in aqueous salt solution
WO2005009578A2 (en) * 2003-07-16 2005-02-03 Amalgamated Research, Inc. Method for the recovery of acids from hydrometallurgy process solutions
CN100999364A (en) * 2006-05-16 2007-07-18 葛文宇 Comprehensive utilization high advantage zero discharge seawater desalination production technology
CN101850991A (en) * 2010-01-14 2010-10-06 河北工业大学 Method for preparing potassium chloride from seawater

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107285430A (en) * 2016-04-05 2017-10-24 亚太森博(山东)浆纸有限公司 A kind of salt dissolving pond, chlor-alkali salt water treating system and chlor-alkali saline treatment technique
CN108996521A (en) * 2018-08-07 2018-12-14 泉州师范学院 A kind of technique using the selective electrodialysis concentration high-purity purified salt of brine production
CN108996521B (en) * 2018-08-07 2021-03-26 泉州师范学院 Process for producing high-purity refined salt by using selective electrodialysis concentrated brine
CN112723388A (en) * 2020-12-25 2021-04-30 卢广荣 Preparation method of medical potassium-free micro-sodium salt

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