CN110436482A - A kind of method of high potassium/sodium in removal ammonium chloride mother liquor - Google Patents
A kind of method of high potassium/sodium in removal ammonium chloride mother liquor Download PDFInfo
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- CN110436482A CN110436482A CN201910741513.0A CN201910741513A CN110436482A CN 110436482 A CN110436482 A CN 110436482A CN 201910741513 A CN201910741513 A CN 201910741513A CN 110436482 A CN110436482 A CN 110436482A
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- sodium
- mother liquor
- ammonium chloride
- potassium
- ammonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
Abstract
The invention discloses a kind of methods of high potassium/sodium in removal ammonium chloride mother liquor: using high potassium/sodium ammonium chloride mother liquor as stoste, using ion-exchange, it is swapped out kalium ion and natrium ion from high potassium/sodium ammonium mother liquor with ammonium type ion exchange resin, to remove high potassium/sodium in ammonium chloride mother liquor, obtains low potassium and sodium ammonium mother liquor；Low potassium and sodium ammonium mother liquor returns to the Production of Ammonium Chloride circulatory system, produces the ammonium chloride product of different purity rank.Hydrochloric acid and ammonium hydroxide are only introduced during processing method of the invention, not newly-increased any one may introduce the novel chemical substance of impurity, not will cause chemical reagent systemic contamination to ammonium chloride mother liquor, will not influence the quality of the ammonium chloride of production.The every wheel of processing method of the invention only handles the high potassium/sodium ammonium chloride mother liquor of 1 times of resin volume, and potassium sodium removal rate is up to 60% or more, and the high potassium/sodium ammonium chloride mother liquor of 2 times of resin volumes of every wheel processing, potassium sodium removal rate is up to 30% or more.
Description
Technical field
The present invention relates to the processing methods of industrial ammonium chloride mother liquor, specifically refer to high potassium in a kind of removal ammonium chloride mother liquor
The method of sodium.
Background technique
Ammonium chloride mother liquor removes there are four types of the methods of potassium sodium, is respectively as follows: organic solvent extractionprocess, chemical addition agent removal of impurities
Method, ion-exchange, the ion exchange method of exclusion.
Organic solvent extractionprocess goes the mechanism of potassium sodium, is that crown compound will not be complexed to be transferred to water phase, alkali gold from organic phase
Belong to and being complexed with crown compound in water phase, ion pair is formed in water phase by complex cation and anion, complex ion is by water phase
Into organic phase, to reach deimpurity purpose.The method is very strong except impurity selectivity, and extraction efficiency is also high.Major defect is
Cave ether expensive, manufacturer is few, is not easy to purchase, and new chemical substance is introduced in ammonium chloride circulating system, easily causes
New systemic contamination.
Chemical addition agent impurity removal method removes potassium sodium, which removes kalium ion and natrium ion by addition chemical reagent, and environmental protection pressure is big, and
New chemical substance is introduced in ammonium chloride circulating system, easily causes new systemic contamination.
Ion-exchange removes potassium sodium, which be used to isolate kalium ion and natrium ion in Reagent-level Ammonium Chloride production process: first use
Sodium form resin is converted h type resin by twice of resin volume dilute hydrochloric acid, then is regenerated after pillar with ammonium hydroxide wash with distilled water
It is converted into monium resin, industrial ammonium chloride dissolution is then made to 30% solution, monium resin tower is flowed through after removal of impurities, is swapped out
Kalium ion and natrium ion, obtains ammonium chloride with low potassium and sodium solution, and condensing crystallizing reagent preparation grade ammonium chloride finally makes resin wash with distilled water
Tower, into next circulation.Although the method removes potassium, sodium effect is preferable, and without introducing new chemical substance, will not be to ammonium chloride
Production system pollutes, but the technique is gap method, and a certain amount of remaining waste liquid, and ion exchange can be generated after condensing crystallizing
The wastewater flow rate generated in the process is big, and about 8 times of resin volume waste water, processing difficulty is big, and environmental protection pressure is big, and ammonia volume is larger,
It is volatile, it is toxic, it can not recycle and reuse, it is at high cost, it operates and also bothers, therefore should not use.In addition, ion exchange
Method is also applied to the separation of ammonium chloride double salt body, prepares ammonium chloride with low potassium and sodium.The method first step uses ion-exchange, destroys
Ammonium chloride double salt body, ammonium chloride mother liquor flow through monium resin tower, when potassium concentration is reduced to 1 ‰ in solution, chlorination
The double salt body of potassium ammonium no longer exists, condensing crystallizing, obtains industrial grade ammonium chloride, and potassium type resin uses the aqueous solution of ammonium sulfate to regenerate again
At monium resin；Industrial grade ammonium chloride containing a certain amount of kalium ion and natrium ion is dissolved in water and saturated solution is made, chlorine is added by second step
To change barium and removes sulfate, chlorine dioxide removes iron, and it adds except potassium sodium additives, precipitates, filter, cool down, crystallization, by handling again
Afterwards to get arrive low potassium and sodium grade ammonium chloride.The ion-exchange of method application is for destroying ammonium chloride double salt body, therefore friendship
Kalium ion and natrium ion residual quantity after changing is bigger, needs further to add except potassium sodium additives chemical reagent removing kalium ion and natrium ion,
Systemic contamination is increased, and the method uses ammonium sulfate as actified solution, is only applicable to ammonium sulfate and potassium chloride metathesis reaction
In the production system of preparing potassium sulfate, such ammonium sulfate can return to the recycling of original production system.For common ammonium chloride
Mother liquor purification system is simultaneously not suitable for, and be will increase sulfate ion pollution, is increased the trouble of removal of impurities.In addition, the ion exchange of the method
Process is only to exchange between potassium ion and ammonium ion, does not use dilute hydrochloric acid and elutes this step, although the selection of potassium ion
Property be greater than ammonium ion, but the two difference is little, and ion-exchanging efficiency is not high, can not accomplish efficiently to remove potassium sodium, therefore only fit
For destroying ammonium chloride double salt body.
The ion exchange method of exclusion removes potassium sodium, which exactly leads to one kind containing electrolyte together with the solution of weak (non-) electrolyte
Ion exchange column is crossed, if wherein the ion identical with symbol in electrolyte of the exchangeable ion in resin is of the same race, is set at this time
Exchange reaction does not occur for rouge, and only electrolyte is repelled away, but weak (non-) electrolyte is because having some affinities with resin
Power and be delayed by outflow, make electrolyte and method that weak (non-) electrolyte is efficiently separated.By K, Na in ammonium chloride solution
Ion selectivity is converted to ionic associate, using conventional ion exchange technique isolated from ammonium chloride solution K, Na from
Son.The method goes potassium sodium effect fine, and K, Na ion can be removed in depth, but needs to turn using ammonium hydrogen carbonate, ammonium hydroxide and crown ether
Agent introduces new chemical substance in ammonium chloride circulating system, easily causes new systemic contamination, while generating a large amount of waste water, energy
Consumption and environmental protection pressure are big.
Summary of the invention
The purpose of the present invention is overcoming the shortcomings of to mention in background above technology and defect, provide a kind of low consumption, efficiently, nothing
The method of high potassium/sodium, the ammonium chloride product of different purity rank easy to produce in the few removal ammonium chloride mother liquor of pollution, wastewater flow rate.
In order to solve the above technical problems, technical solution proposed by the present invention are as follows:
The method of high potassium/sodium is handed over using high potassium/sodium ammonium chloride mother liquor as stoste using ion in a kind of removal ammonium chloride mother liquor
Method is changed, is swapped out kalium ion and natrium ion from high potassium/sodium ammonium mother liquor with ammonium ion exchanger resin, to remove high potassium/sodium in ammonium chloride mother liquor,
Obtain low potassium and sodium ammonium mother liquor；
Wherein, the method for removing high potassium/sodium in ammonium chloride mother liquor includes the following steps:
(1) by high potassium/sodium ammonium chloride mother liquor to be processed by be equipped with ammonium type ion exchange resin exchange column, ammonium type from
Ammonium ion in sub-exchange resin is exchanged by kalium ion and natrium ion into mother liquor, ammonium type ion exchange resin be transformed into potassium sodium form from
Sub-exchange resin；High potassium/sodium ammonium chloride mother liquor is transformed into low potassium and sodium ammonium mother liquor；
(2) the potassium sodium form ion exchange resin is excessively first eluted with dilute hydrochloric acid, is then obtained wash with distilled water to neutrality
To form ion exchange resin, then regenerated to obtain ammonium type ion exchange resin with ammonium chloride solution；
(3) the ammonium type ion exchange resin for obtaining regeneration carries out high potassium/sodium ammonium chloride mother liquor by the method for step (1) again
Processing, realize high potassium/sodium ammonium chloride mother liquor circular treatment.
Wherein preferably, the ammonium type ion exchange resin in step (1) is prepared by following methods:
S1: sodium form ion exchange resin is packed into ion exchange column, is excessively eluted with dilute hydrochloric acid, by sodium form ion exchange
Resin is converted to form ion exchange resin；
S2: being passed through in ion exchange column with distilled water, and form ion exchange column is cleaned to neutrality；
Ammonium chloride solution: being passed through in ion exchange column by S3 again, by the form ion exchange resin be converted into ammonium type from
Sub-exchange resin.
Preferably, the sodium form ion exchange resin is 732 type sodium form resins.
Preferably, in step (1), the volume of the high potassium/sodium ammonium chloride mother liquor handled each time is ammonium type ion exchange resin
0.5-3 times of volume.
Preferably, dilute hydrochloric acid is the hydrochloric acid solution of 0.5-2mol/L.
Preferably, the mass fraction of ammonium chloride solution is 5-10%.
Preferably, in the high potassium/sodium ammonium chloride mother liquor, potassium concentration 110-140ppm, Na ion concentration is
23000-28000ppm；In the low potassium and sodium ammonium mother liquor, potassium concentration 35-100ppm, Na ion concentration 6000-
17000ppm。
Preferably, the low potassium and sodium ammonium mother liquor returns to the Production of Ammonium Chloride circulatory system, produces the chlorination of different purity rank
Ammonium product.
Preferably, the Production of Ammonium Chloride circulatory system refers to, raw by recrystallization method impurity elimination using industrial ammonium chloride as raw material
Produce the process of the ammonium chloride product of different purity rank, concrete technology flow process are as follows: industrial ammonium chloride is put into circulation saturation chlorine
To change in ammonium mother liquor, obtains solidliquid mixture, high-temperature digestion filters, and it is cooling, it recrystallizes, centrifugation, isolated different purity rank
Ammonium chloride product, while the saturated ammonium chloride mother liquor that centrifugation obtains, for the Production of Ammonium Chloride process of next batch, when saturation chlorine
Change potassium sodium content in ammonium mother liquor to reach a certain height, cannot be further continued in use, reducing its potassium sodium using the method for the invention
After content, use can be continued cycling through.
Preferably, the dilute hydrochloric acid excessively elutes, and refers to that column stream eluent is changed into 1 acid boundary's point by neutrality, at this time
It is clean that the kalium ion and natrium ion adsorbed on ion exchange column also remains more incomplete elution, therefore elution process at this time can not
It terminates, needs to continue excessively to be eluted with dilute hydrochloric acid, until column stream eluent is substantially free of kalium ion and natrium ion through detection, Cai Nengjin
Row next step distilled water cleaning step.
Preferably, liquid solution (including ammonium chloride mother liquor, dilute hydrochloric acid, ammonium chloride solution distilled water etc.) passes through ion exchange
Column linear velocity when column is 10-20m/h.
The present invention carries out ion exchange by way of not introducing novel chemical substance, carries out recycling to resin,
To reduce the concentration of potassium, sodium in high potassium/sodium ammonium chloride mother liquor.
The principle of the invention lies in the concentration for reducing potassium, sodium in high potassium/sodium ammonium chloride mother liquor, so the present invention is to potassium, sodium
Concentration does not require particularly.
Easy for statement, by " potassium sodium form ion exchange resin " abbreviation " potassium sodium form resin " in the present invention, " ammonium type ion is handed over
Change resin " abbreviation " monium resin ", it omits " ion exchange resin " therein, and so on.
In the present invention, the volume that nature is filled in ion exchange column is subject in the measurement of resin volume.
Compared with the prior art, the advantages of the present invention are as follows:
(1) hydrochloric acid and ammonium hydroxide have been only introduced during processing method of the invention, not newly-increased any one may introduce
The novel chemical substance of impurity not will cause chemical reagent systemic contamination to ammonium chloride mother liquor, will not influence the ammonium chloride of production
Quality.
(2) the every wheel of processing method of the invention only handles the high potassium/sodium ammonium chloride mother liquor of 1 times of resin volume, potassium sodium removal rate
It is up to 60% or more, the high potassium/sodium ammonium chloride mother liquor of 2 times of resin volumes of every wheel processing, potassium sodium removal rate is up to 30% or more.
(3) water circulation use rate is high during processing method of the invention, substantial saved water resource, reduces costs,
And the wastewater flow rate for needing to discharge is few, only 1.2 times of resinite accumulated amounts, wastewater treatment qualified discharge is also very simple.
(4) present invention is excessively eluted with dilute hydrochloric acid, the kalium ion and natrium ion being adsorbed on ion column is eluted substantially, this is
One important discovery of this method, in addition most dilute hydrochloric acid recycles, and can preferably reduce cost.
(5) present invention uses ammonium chloride solution as regenerated liquid and recycles, and not only safe ready but also has reduced costs.
(6) low energy consumption for processing system of the invention, does not consume thermal energy, need to only consume a small amount of electric energy.
Detailed description of the invention
Fig. 1 is process flow diagram of the invention.
Specific embodiment
To facilitate the understanding of the present invention, invention herein is done below in conjunction with Figure of description and preferred embodiment more complete
Face meticulously describes, but protection scope of the present invention is not limited to following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter are generally understood meaning phase with those skilled in the art
Together.Technical term used herein is intended merely to the purpose of description specific embodiment, and it is of the invention to be not intended to limitation
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1:
732 sodium form ion exchange resin are packed into ion exchange column as shown in Figure 1:, it is excessive with 1.6mol/L dilute hydrochloric acid
Sodium form resin is converted to h type resin by the flow velocity of column linear velocity 15m/h by exchange column by elution, in elution process, front
Point middle acidic effluent liquid waste water flow into wastewater trough after simple neutralisation treatment can direct emission, the acidic elution liquid stream of rear part
Enter diluted acid circulation underground tank to recycle；Dilute hydrochloric acid remaining in exchange column is cleaned up to neutrality with distilled water again, is steamed
Distilled water cleaning solution all flows into distilled water reuse slot and recycles for preparing dilute hydrochloric acid, and the ammonium chloride with mass fraction 8% is molten
Liquid crosses column regeneration, i.e., h type resin is converted into monium resin, obtains ammonium ion exchange column and acid chlorization ammonium salt solution, acid chlorine
Change ammonium salt solution and all flow into ammonium chloride circulation underground tank, is recycled after being neutralized with a small amount of concentrated ammonia liquor.
The high potassium/sodium ammonium chloride mother liquor of 1 times of resin volume is passed through into ammonium ion exchange column by the flow velocity of column linear velocity 15m/h,
Kalium ion and natrium ion in ammonium mother liquor is adsorbed by monium resin, is converted into potassium sodium form resin, and the ammonium ion being swapped out enters ammonium mother liquor, ammonium
Ammonium concentration in mother liquor increases, and kalium ion and natrium ion concentration reduces, and obtained low potassium and sodium ammonium mother liquor returns Production of Ammonium Chloride and follows
In loop system, and then produce the ammonium chloride product of different purity rank.
Potassium sodium form resin is excessively eluted with dilute hydrochloric acid, clean to neutrality wash with distilled water, obtains h type resin, then use
Ammonium chloride solution regeneration, obtains monium resin, carries out the circular treatment high potassium/sodium ammonium chloride mother liquor of next round.
After testing, the high potassium/sodium ammonium chloride mother liquor of 1 times of resin volume of every wheel processing, the total dosage of dilute hydrochloric acid are 3 times of resins
Volume, the distillation water consumption of cleaning pillar are 1.2 times of resin volumes, and wastewater discharge is 1.2 times of resin volumes, high potassium/sodium chlorine
Change in ammonium mother liquor, potassium concentration 130ppm, Na ion concentration 25000ppm, after processing, potassium concentration is reduced to
50ppm, Na ion concentration are reduced to 8250ppm, and potassium removal rate is up to 62%, and sodium removal rate is up to 67%.
Embodiment 2:
The step of embodiment 2 is with embodiment 1 is identical, and difference is only that: the body of the high potassium/sodium ammonium chloride mother liquor of every wheel processing
Product is 2 times of the resin volume in ion exchange column.After tested, in high potassium/sodium ammonium chloride mother liquor, potassium concentration 130ppm,
Na ion concentration is 25000ppm, and after processing, potassium concentration is reduced to 78ppm, and Na ion concentration is reduced to 14000ppm, and potassium is gone
Except rate is up to 40%, sodium removal rate is up to 44%.
Embodiment 3:
The step of embodiment 3 is with embodiment 1 is identical, and difference is only that: excessively being eluted with 0.8mol/L dilute hydrochloric acid, dilute hydrochloric acid
Total dosage is 4 times of resin volumes.After tested, in high potassium/sodium ammonium chloride mother liquor, potassium concentration 130ppm, Na ion concentration is
25000ppm, after processing, potassium concentration is reduced to 45ppm, and Na ion concentration is reduced to 6750ppm, and potassium removal rate is up to 65%,
Sodium removal rate is up to 73%.
Embodiment 4:
The step of embodiment 4 is with embodiment 1 is identical, and difference is only that: excessively being eluted with 0.8mol/L dilute hydrochloric acid, dilute hydrochloric acid
Total dosage is 4 times of resin volumes, and the volume of the high potassium/sodium ammonium chloride mother liquor of each round processing is the resinite in ion exchange column
Long-pending 2 times.After tested, in high potassium/sodium ammonium chloride mother liquor, potassium concentration 130ppm, Na ion concentration 25000ppm, place
After reason, potassium concentration is reduced to 88ppm, and Na ion concentration is reduced to 14750ppm, and for potassium removal rate up to 32%, sodium removal rate can
Up to 41%.
Claims (9)
1. a kind of method of high potassium/sodium in removal ammonium chloride mother liquor, which is characterized in that using high potassium/sodium ammonium chloride mother liquor as stoste, adopt
With ion-exchange, it is swapped out kalium ion and natrium ion from high potassium/sodium ammonium mother liquor with ammonium type ion exchange resin, to remove ammonium chloride mother
High potassium/sodium in liquid obtains low potassium and sodium ammonium mother liquor；
Wherein, the method for removing high potassium/sodium in ammonium chloride mother liquor includes the following steps:
(1) by high potassium/sodium ammonium chloride mother liquor to be processed by the exchange column equipped with ammonium type ion exchange resin, ammonium type ion is handed over
The ammonium ion changed in resin is exchanged by kalium ion and natrium ion into mother liquor, and ammonium type ion exchange resin is transformed into the friendship of potassium sodium form ion
Change resin；High potassium/sodium ammonium chloride mother liquor is transformed into low potassium and sodium ammonium mother liquor；
(2) the potassium sodium form ion exchange resin is excessively first eluted with dilute hydrochloric acid, then obtains hydrogen to neutrality wash with distilled water
Type ion exchange resin, then regenerated to obtain ammonium type ion exchange resin with ammonium chloride solution；
(3) the ammonium type ion exchange resin for obtaining regeneration is carried out the place of high potassium/sodium ammonium chloride mother liquor by the method for step (1) again
Reason realizes the circular treatment of high potassium/sodium ammonium chloride mother liquor.
2. the method according to claim 1, wherein the ammonium type ion exchange resin in step (1) is by with lower section
Method is prepared:
S1: sodium form ion exchange resin is packed into ion exchange column, is excessively eluted with dilute hydrochloric acid, by sodium form ion exchange resin
Be converted to form ion exchange resin；
S2: being passed through in ion exchange column with distilled water, and form ion exchange column is cleaned to neutrality；
Ammonium chloride solution: being passed through in ion exchange column by S3 again, and the form ion exchange resin is converted into ammonium type ion and is handed over
Change resin.
3. according to the method described in claim 2, it is characterized in that, the sodium form ion exchange resin is 732 type sodium form resins.
4. method according to claim 1-3, which is characterized in that in step (1), the high potassium/sodium that handles each time
The volume of ammonium chloride mother liquor is 0.5-3 times of ammonium type ion exchange resin volume.
5. method according to claim 1-3, which is characterized in that the dilute hydrochloric acid is the salt of 0.5-2mol/L
Acid solution.
6. method according to claim 1-3, which is characterized in that the mass fraction of the ammonium chloride solution is
5-10%.
7. method according to claim 1-3, which is characterized in that in the high potassium/sodium ammonium chloride mother liquor, potassium from
Sub- concentration is 110-140ppm, Na ion concentration 23000-28000ppm；In the low potassium and sodium ammonium mother liquor, potassium concentration is
35-100ppm, Na ion concentration 6000-17000ppm.
8. method according to claim 1-3, which is characterized in that it is raw that the low potassium and sodium ammonium mother liquor returns to ammonium chloride
The circulatory system is produced, the ammonium chloride product of different purity rank is produced.
9. method according to claim 1-3, which is characterized in that liquid solution passes through column when ion exchange column
Linear velocity is 10-20m/h.
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| CN112121873A (en) * | 2020-09-21 | 2020-12-25 | 昆山三一环保科技有限公司 | Regeneration process of cobalt-removing resin |
| CN112142068A (en) * | 2020-09-07 | 2020-12-29 | 湖北兴福电子材料有限公司 | Method for producing high-purity ammonium chloride from industrial-grade ammonium chloride |
| CN113634014A (en) * | 2021-08-17 | 2021-11-12 | 新乡赛普瑞特环保科技有限公司 | System and method for separating potassium ions in lithium solution |
| CN115779983A (en) * | 2022-10-24 | 2023-03-14 | 天津市中医药研究院附属医院 | Ion exchange technology-based traditional Chinese medicine decoction potassium removal process |
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2019
- 2019-08-12 CN CN201910741513.0A patent/CN110436482A/en active Pending
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112142068A (en) * | 2020-09-07 | 2020-12-29 | 湖北兴福电子材料有限公司 | Method for producing high-purity ammonium chloride from industrial-grade ammonium chloride |
| CN112121873A (en) * | 2020-09-21 | 2020-12-25 | 昆山三一环保科技有限公司 | Regeneration process of cobalt-removing resin |
| CN112121873B (en) * | 2020-09-21 | 2023-06-09 | 昆山三一环保科技有限公司 | Regeneration process of cobalt-removing resin |
| CN113634014A (en) * | 2021-08-17 | 2021-11-12 | 新乡赛普瑞特环保科技有限公司 | System and method for separating potassium ions in lithium solution |
| CN115779983A (en) * | 2022-10-24 | 2023-03-14 | 天津市中医药研究院附属医院 | Ion exchange technology-based traditional Chinese medicine decoction potassium removal process |
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Application publication date: 20191112 |