CN105600805B - A kind of method that ammonium sulfate is isolated and purified in the regenerative process by-product solution from fume desulfurizing agent - Google Patents
A kind of method that ammonium sulfate is isolated and purified in the regenerative process by-product solution from fume desulfurizing agent Download PDFInfo
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- CN105600805B CN105600805B CN201610038217.0A CN201610038217A CN105600805B CN 105600805 B CN105600805 B CN 105600805B CN 201610038217 A CN201610038217 A CN 201610038217A CN 105600805 B CN105600805 B CN 105600805B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
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- C01—INORGANIC CHEMISTRY
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- C01P2006/80—Compositional purity
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Abstract
A kind of method that ammonium sulfate is isolated and purified in regenerative process by-product solution from fume desulfurizing agent, by NH4 +Type cationic ion-exchange resin is filled in cation exchange column using wet method, by sodium acid carbonate regeneration accessory substance mixed solution by resin bed, collects post bottom ammonium sulfate and ammonium hydrogen carbonate efflux；By efflux after dilute sulfuric acid is acidified and dries, ammonium sulfate is obtained, complete to isolate and purify；The ion exchange resin failed in exchange column is filled in using deionized water, ammonium bicarbonate soln, deionized water priority drip washing to be regenerated, and NH can be obtained again4 +Type resin.Present invention introduces ion exchange resin, Efficient Conversion in sodium acid carbonate regenerative process accessory substance mixed solution is purified and is acidified so as to obtain high-purity sulfuric acid ammonium, and loaded resin is utilized by being repeated after regeneration, resin regeneration efflux can also continue to serve as desulfurizing agent, without waste residue and liquid discharge, the green economy and utilization rate of technique are improve, rational approach is provided to reclaim.
Description
Technical field
Technical field is utilized the invention belongs to industrial wastewater, and in particular to a kind of from fume desulfurizing agent regenerative process accessory substance
The method that ammonium sulfate is isolated and purified in solution.
Background technology
The atmosphere pollution of current China is increasingly serious, used as maximum in the world coal production state and country of consumption, sulfur dioxide
Total emission volumn is in world's umber one, and in this context, flue gas desulfurization technique has obtained fast development in recent years, but largely
Desulfurizing byproduct it is also following, for traditional limestone-gypsum method, China just produces desulfurated plaster 5230 in only 2010
Ten thousand tons, desulfurated plaster comprehensive utilization it is poor, at this stage mainly with abandon stack based on, both waste land resource, again produce ring
Pollute in border.Therefore, the accessory substance produced by desulphurization denitration process process is put in face of chemical industry and environmentalist
Very urgent task.
Sodium acid carbonate sulfur method is than traditional desulfurization method of limestone-gypsum rate (close to 100% removal efficiency) high, reaction speed
Rate is fast, alkali utilization rate is high, and can simultaneously remove the heavy metals such as nitrogen oxides and mercury, and Tongji University's Dongmei SUN exists《Sodium acid carbonate
Desulfurization and its screening of optimal conditions are inquired into》And Timothy C.Keener exist《Study of the Reaction of
SO2with NaHCO3and Na2CO3》In mention NaHCO3Typically there is preferable desulfurized effect under different shape, there is pole
Great development utilizes future.But two large problems, i.e. cost of material process problem high and accessory substance are faced, sodium acid carbonate suction is constrained
Agent is received in the industrial development of desulfurization, its advantage is not brought into play at utmost.NaHCO3Flue gas desulfurization primary chemical is anti-
Should be：2NaHCO3+SO2+1/2O2→Na2SO4+2CO2+H2O, 2NaHCO3→Na2CO3+CO2+H2O, Na2CO3+SO2+1/2O2→
Na2SO4+2CO2。
In order to reduce cost and by-product contamination, " The Airborn ProcessTM" take ten years and work out
A whole set of sodium acid carbonate removing SO2(US 005980848A, US 7393378B2), sodium acid carbonate regeneration (US 6475458B)
And regeneration accessory substance fertilizer purifies technology and the SEPARATE APPLICATION of (US 006106796A) patent, and in the willing tower of U.S.'s Gent
Ji Zhou (Airborn companies 5MW power plants demonstration project), the Wyoming State (Jim Bridger power plants) and Haier of West Germany cloth are grand
The input application such as (Solvary power plants) ground.Sodium acid carbonate regenerative process main chemical reactions equation is：NH4HCO3+
Na2SO4→(NH4)2SO4+NaHCO3↓, i.e., more expensive sodium acid carbonate is regenerated come NaHCO with cheap ammonium hydrogen carbonate3Crystallization
Contain Na in residual solution afterwards2SO4、(NH4)2SO4、NH4HCO3With a small amount of NaHCO3If directly discharge will cause this waste water
This waste water is acidified gained ammonium sulfate and the double salting liquids of sodium sulphate by serious water pollution, Airborn by dilute sulfuric acid, it is further contemplated that
The economic worth of sodium sulphate is limited in this waste water, so this waste water is carried out into separating-purifying, obtains high-purity sulfuric acid ammonium, sulfuric acid
Ammonium can be used as nitrogenous fertilizer, ore floatation, metal recovery, production refractory material etc., so that larger economic benefit can be obtained, by 6
Year (1990~1996) time process optimization, the purity of ammonium sulfate is brought up to 99% by it with Steppecd crystallization from 60%, point
Separate out the sodium sulphate for coming and again return to sodium acid carbonate regeneration stage.The method is high to Control system resolution requirement, expend heat energy, crystallization
Effectively control is difficult with sweating speed, recyclability is not strong.
The content of the invention
To overcome the problems of the prior art, it is an object of the invention to provide a kind of selectivity it is good, can be recycled, environment
Pollution less, be suitable to industrialized production, low cost and from fume desulfurizing agent regenerative process by-product solution isolate and purify ammonium sulfate
Method.
To achieve these goals, the present invention is adopted the following technical scheme that：
A kind of method that ammonium sulfate is isolated and purified in regenerative process by-product solution from fume desulfurizing agent, by NH4 +Type sun from
Sub-exchange resin is filled in cation exchange column using wet method, at room temperature, fume desulfurizing agent regenerative process accessory substance is mixed
Solution is by resin bed, the Na in the accessory substance mixed solution of fume desulfurizing agent regenerative process generation+With the NH on resin4 +Hair
Raw exchange reaction, collects post bottom efflux, with the Na in efflux+Concentration reaches 5mg/L to collect terminal；The outflow that will be collected
After liquid is acidified to pH value for 4~5 and drying through persulfuric acid, ammonium sulfate is obtained, complete to isolate and purify.
The NH4 +Type cationic ion-exchange resin is containing sulfonic resin.
Described is gel-network precipitation method Seplite LSI-010, macroporous type cation containing sulfonic resin
Exchanger resin Amberlite FPC22Na or Amberlite 252Na.
The flow velocity that the fume desulfurizing agent regenerative process accessory substance mixed solution passes through resin bed is 2~8BV/h.
By the NH after failure4 +It is 7~9 that type cationic ion-exchange resin is first washed with deionized to efflux pH value, then
With ammonium bicarbonate soln, ammonium chloride solution or ammonium sulfate drip washing resin, finally it is washed with deionized to efflux pH value
It is 7~9, obtains NH4 +Type cationic ion-exchange resin, NH4 +Type cationic ion-exchange resin can be reused.
The molar concentration of the ammonium bicarbonate soln, ammonium chloride solution or ammonium sulfate is 1~2mol/L, ammonium hydrogen carbonate
The volume of solution, ammonium chloride solution or ammonium sulfate is 3~5BV.
By the NH after failure4 +When type cationic ion-exchange resin is first washed with deionized, the flow velocity of deionized water used is 6
~8BV/h.
The flow velocity of the ammonium bicarbonate soln, ammonium chloride solution or ammonium sulfate is 1.5~2BV/h.
Compared with prior art, the device have the advantages that as follows：The present invention at room temperature, uses NH4 +Type cation
Exchanger resin carries out ion-exchange reactions to fume desulfurizing agent regenerative process by-product solution and efflux to be acidified to pH value be 4
~5 and dry, obtain high-purity sulphuric acid ammonium, with simplicity, purification efficiency advantage high, resin repeats regeneration, and sets
Fat regenerative process efflux can also continue to serve as desulfurizing agent, and the ammonium sulfate purity obtained by the method reaches more than 97%, tool
There is actual application value higher, solve sodium acid carbonate in the prior art and deposited in being processed as desulfurizer regeneration process byproduct
Difficult manipulation, the too big problem of energy consumption, the present invention greatly reduces production cost, compensate for sodium acid carbonate method desulphurization cost high
Shortcoming, other foreign ions will not be introduced again, reduce water pollution, without waste residue and liquid discharge, comprehensive resource utilization rate it is high,
Selectivity is good, and the green economy of whole method is good, provides rational approach to reclaim valuable industry and product for agriculture, more
Large-scale use for sodium acid carbonate method in flue gas desulfurization field provides possibility.For containing ammonium ion and sodium ion in solution
Mixed liquor, anion be other ions, such as carbanion, chlorion, bicarbonate radical etc., equally can using the present invention
In method purified.
Further, the resin after ion exchange can carry out regeneration cycle with ammonium bicarbonate soln or other ammonium salt solutions
Utilize, regenerative process efflux can continue to serve as desulfurizing agent or recycling, and resin repeat usage is high.
Further, if using ammonium sulfate regenerating resin, efflux is double salt sodium sulphate and ammonium sulfate mixed solution, is somebody's turn to do
Mixed solution can return to deionization and exchange and be acidified obtain ammonium sulfate again, and the ammonium sulfate of regeneration comes to desulfurizing byproduct
The ammonium sulfate that solion is exchanged and obtained after being acidified.This is also a circulation.
Brief description of the drawings
Fig. 1 is the schematic diagram that exchange adsorption is carried out on ion exchange resin.
Specific embodiment
The present invention is explained in detail in by the way of specific embodiment below, but the present invention is not limited to embodiment.This hair
The concentration of bright middle sulfuric acid is 0.1mol/L.
The present invention is comprised the following steps：
1) by NH4 +Type cationic ion-exchange resin is filled in cation exchange column using wet method, at room temperature, by flue gas desulfurization
Agent regenerative process by-product solution (i.e. sodium acid carbonate desulfurization regeneration accessory substance mixed solution, Na2SO4、(NH4)2SO4、NH4HCO3
With a small amount of NaHCO3) resin bed, Na in fume desulfurizing agent regenerative process by-product solution are passed through with the flow velocity of 2~8BV/h+With
The NH combined on resin4 +Generation exchange reaction, collects post bottom efflux, with the Na in efflux+Concentration reaches 5mg/L for eventually
Point, stops collecting.
2) ammonium sulfate and ammonium hydrogen carbonate are included in efflux, it is 4 that the efflux of collection is acidified into pH value by dilute sulfuric acid
~5 and dry after, obtain ammonium sulfate, complete to isolate and purify；Wherein, BV is resin volume.
3) cationic ion-exchange resin after failure is filled in exchange column using wet method, deionized water is used first with 6
It is 7~9 that~8BV/h is washed to efflux pH value, then with the ammonium bicarbonate soln that 3~5BV, molar concentration are 1~2mol/L
With the speed drip washing resin of 1.5~2BV/h, it is 7~9 finally to be washed to efflux pH value with 6~8BV/h with deionized water, is obtained
To NH4 +Type cationic ion-exchange resin, the NH4 +Cation exchange groups contained by type cationic ion-exchange resin are, containing sulfonic resin, to contain
The resin of benzene sulfonic acid base can equally be used.
The use ammonium bicarbonate soln drip washing resin, efflux is that sodium acid carbonate and ammonium hydrogen carbonate mixed solution can continue to use
Make fume desulfurizing agent.Ammonium bicarbonate soln can also use the ammonium salts such as ammonium chloride solution, ammonium sulfate to replace, but now, efflux
It is exactly villaumite or sulfate liquor, also recyclable conversion is recycled.The purpose that sulfuric acid is used in the present invention is acidifying, and its concentration is not
It is restricted.
The present invention is described in detail below：
The first step, the type selecting of resin：According to the characteristic of ion exchange resin, in conjunction with the sodium acid carbonate for being currently needed for purifying
The property and feature of desulfurization regeneration accessory substance mixed solution, from storng-acid cation exchange resin, with reference to itself system and
The use parameter and performance of resin, the NH of final choice4 +Type cationic ion-exchange resin be containing cation exchange groups be sulfonic group or benzene sulphur
The resin of acidic group.
Second step, conversion purification ammonium sulfate：Using NH4 +Type cationic ion-exchange resin and Na in solution+Swap reaction,
And to efflux be acidified to pH and be 4~5, dry so as to obtain the ammonium sulfate of high-purity, specifically, by NH4 +Type sun
Ion exchange resin wet method is filled in cation exchange column, at room temperature, sodium acid carbonate desulfurization regeneration byproduct in process thing is mixed
Solution is closed with the flow velocity of 2~8BV/h by resin bed, so that the Na in liquid phase+From liquid phase bulk motion to resin particle table
Face, and with the NH that combines on resin4 +Generation exchange reaction, the NH got off by exchange4 +It is diffused into liquid phase main body so that in solution
Only NH4 +.Whole exchange process both occurs to be also occurred in inside resin in resin surface, and follows equivalent exchange principle, instead
Ying Shiwei 2R-NH4+Na2SO4→2R-Na+(NH4)2SO4, R-NH4+NaHCO3→R-Na+NH4HCO3.The schematic diagram of exchange adsorption
See Fig. 1, in ion exchange process, what the function base being connected on the changeless skeleton in ion exchange resin was dissociated
Ammonium ion is swapped with the sodium ion dissociated in solution, and whole exchange process follows equivalent and exchanges principle, and in resin
Particle surface and inside all there occurs ion exchange process, thus in solution ammonium ion amount increase, collect post bottom ammonium sulfate with
Ammonium hydrogen carbonate efflux.Under normal circumstances, the speed of Liquid film diffusion or particles diffusion determines the general speed of ion exchange.
Finally press formula Q=(C-C0) V/W converses the ion exchange capacity of ion exchange resin under fixed mass.
In formula：Q—Na+Exchange capacity；
C0NH in-solution4 +Initial concentration (mg/L)；
NH in C-exchange efflux4 +Concentration (mg/L)；
V-effluent volume (L)；
The quality (g) of W-isolate and purify institute's spent ion exchange resin；
3rd step, the transition of resin：The resin of gained after step 2 conversion purification is filled in exchange column using wet method,
Use first deionized water with the flow velocity washing resin of 6~8BV/h to efflux pH value be 7~9, then using 3~5BV of volume,
Molar concentration be the ammonium bicarbonate soln of 1~2mol/L with the flow velocity drip washing resin of 1.5~2BV/h, sodium form resin is converted into
NH4+ type cationic ion-exchange resin, deionized water is 7~9 with the flow velocity washing resin of 6~8BV/h to efflux pH value, is incited somebody to action
To NH4 +Type storng-acid cation exchange resin is put into standby in closed vessel.
4th step：It is acidified and is dried to obtain ammonium sulfate：Ammonium sulfate obtained by step 2 and ammonium hydrogen carbonate efflux are passed through
Cross dilute sulfuric acid be acidified to pH value for 4~5 and drying after, obtain ammonium sulfate, complete to isolate and purify.Acidifying is placed on by-product solution
After ion exchange, Na can be greatly increased+With NH4 +Between exchange capacity.According to《Measure (the first of nitrogen content in ammonium sulfate fertilizer
Aldehyde method)》To detect the purity of ammonium sulfate.Resulting ammonium sulfate purity is higher than 97%.
It is described in detail below by specific embodiment.Fume desulfurizing agent regenerative process accessory substance in embodiment 1~5
Solution is sodium acid carbonate regenerative process by-product solution.It is 2%, Na that mass concentration is used in embodiment2SO4、(NH4)2SO4、NH4HCO3And NaHCO3Molar concentration rate be 2：4：2：1 mixed solution, ion exchange column volume is 120mL.
Embodiment 1：
1) gel-network precipitation method Seplite LSI-010 are filled in exchange column using wet method, are adopted first
With the flow velocity washing resin of 6BV/h to efflux pH value it is 7~9 with deionized water, is then with volume 4BV, molar concentration
The ammonium bicarbonate soln of 1mol/L finally washs tree with deionized water with the flow velocity of 6BV/h again with 1.5BV/h flow velocity drip washing resins
Fat to efflux pH value is 7~9, obtains NH4 +Type cationic ion-exchange resin.
2) by NH4 +Type cationic ion-exchange resin is filled in cation exchange column using wet method, at room temperature, by flue gas desulfurization
Agent regenerative process by-product solution is with the flow velocity of 3BV/h by resin bed, Na+With the NH combined on resin4 +Generation exchanges anti-
Should, post bottom ammonium sulfate and ammonium hydrogen carbonate efflux are collected, with the Na in efflux+Concentration reaches 5mg/L for terminal, stops receiving
Collection, determines the ion exchange capacity Q of Seplite LSI-010 resins for 20.1mg/g, and the efflux that will be collected is by dilute sulfuric acid
It is 4~5 and after being dried at 55 DEG C in vacuum drying chamber to be acidified to pH value, measures ammonium sulfate purity for 98.2%.
Embodiment 2：Amplification test
1) large pores cation exchange resin Amberlite FPC22Na are filled in exchange column using wet method, first
Use deionized water with the flow velocity washing resin of 8BV/h to efflux pH value be 7~9, then using volume 5BV, molar concentration
It is the ammonium bicarbonate soln of 1.5mol/L with 1.5BV/h flow velocity drip washing resins, is finally washed with the flow velocity of 8BV/h with deionized water again
It is 7~9 to wash resin to efflux pH value, obtains NH4 +Type cationic ion-exchange resin.
2) respectively to wet resin (the i.e. NH of each filling 120mL in two exchange columns4 +Type cationic ion-exchange resin), then by two
Individual exchange column is together in series, by regeneration accessory substance mixed solution with the flow velocity of 2BV/h by resin bed, when second exchange column
Na in efflux+When concentration reaches 5mg/L, stop operation, the resin in two pillars is regenerated, start the pure of second batch
Change experiment, single batch is 20BV or so to the treating capacity for regenerating accessory substance mixed solution, determines first batch FPC22Na resins
Ion exchange capacity Q be 23.8mg/g, it is 4~5 that the ammonium sulfate of collection and ammonium bicarbonate soln are acidified into pH by dilute sulfuric acid
And after drying, it is 99.2% to measure the ammonium sulfate purity of first batch, the exchange capacity Q of second lot is 21.6mg/g, ammonium sulfate
Purity is 98.2%, and the exchange capacity Q of the 3rd batch is 20.8mg/g, and ammonium sulfate purity is 97.5%, the exchange capacity Q of the 4th batch
It is 19.5mg/g, ammonium sulfate purity is 97%, the exchange capacity Q of the 5th batch is 19.1mg/g, and ammonium sulfate purity is 96.5%, is put
Big experiment result shows that resins exchange rate is high, and gained ammonium sulfate purity is high, and absorption property stabilization, the resin after regeneration treatment is inhaled
Attached performance is preferable, keeps adsorption rate higher.
Embodiment 3：
1) large pores cation exchange resin Amberlite FPC 22Na are filled in exchange column using wet method, first
It is 7~9 with the flow velocity washing resin of 6BV/h to efflux pH value to use deionized water, then uses volume for 3BV, mole dense
The ammonium sulfate for 2mol/L is spent with 1.5BV/h flow velocity drip washing resins, is finally washed with the flow velocity of 6BV/h with deionized water again
Resin to efflux pH value is 7~9, obtains NH4 +Type cationic ion-exchange resin.
2) by NH4 +Type cationic ion-exchange resin is filled in cation exchange column using wet method, at room temperature, by flue gas desulfurization
Agent regenerative process regenerates accessory substance mixed solution with the flow velocity of 8BV/h by resin bed, Na+With the NH combined on resin4 +Hair
Raw exchange reaction, collects post bottom efflux, with the Na in efflux+Concentration reaches 5mg/L for terminal, determines Amberlite
The ion exchange capacity Q of FPC22Na resins is 19.1mg/g, and the ammonium sulfate that will be collected is acidified with ammonium bicarbonate soln by dilute sulfuric acid
It is 4~5 to pH, after being dried in 55 DEG C of vacuum drying chambers, it is 97.3% to measure ammonium sulfate purity.
Embodiment 4：
1) large pores cation exchange resin Amberlite 252Na are filled in exchange column using wet method, are adopted first
With the flow velocity washing resin of 7BV/h to efflux pH value it is 7~9 with deionized water, is then 1.5mol/L, body with molar concentration
Product is 5BV, flow velocity is the ammonium chloride solution drip washing resin of 1.8BV/h, finally washs tree with the flow velocity of 6BV/h with deionized water again
Fat to efflux pH value is 7~9, obtains NH4 +Type cationic ion-exchange resin.
2) by NH4 +Type cationic ion-exchange resin is filled in cation exchange column using wet method, at room temperature, by flue gas desulfurization
Agent regenerative process regenerates accessory substance mixed solution with the flow velocity of 6BV/h by resin bed, Na+With the NH combined on resin4 +Hair
Raw exchange reaction, collects post bottom efflux, with the Na in efflux+Concentration reaches 5mg/L for terminal, determines Amberlite
The ion exchange capacity Q of F252Na resins is 19.6mg/g, and the ammonium sulfate that will be collected is acidified with ammonium bicarbonate soln by dilute sulfuric acid
It is 4~5 to pH, after being dried in 55 DEG C of vacuum drying chambers, it is 97.6% to measure ammonium sulfate purity.
For the mixed liquor containing ammonium ion and sodium ion in solution, anion is other ions, such as carbanion,
Chlorion, bicarbonate radical etc., can equally be purified using the method in the present invention.
Existing sodium acid carbonate desulfurization technology cost of material is high and the process problem of accessory substance in order to solve for the present invention, for carbon
Sour hydrogen sodium regenerative process accessory substance mixed solution, carries out conversion purification, and be firstly introduced ion to the ammonium sulfate in mixed solution
Exchanger resin carries out purification process to sodium acid carbonate regenerative process accessory substance mixed solution, and achieves preferable effect, so that
Obtain high-purity sulfuric acid ammonium, develop that a kind of selectivity is good, the rate of recovery is high, can be recycled, it is low in the pollution of the environment, be suitable to industrialization
The ammonium sulfate ion of production exchanges preparation technology, improves the green economy of whole sodium acid carbonate sulfur removal technology.
Claims (1)
1. a kind of method that ammonium sulfate is isolated and purified in regenerative process by-product solution from fume desulfurizing agent, it is characterised in that will
NH4 +Type cationic ion-exchange resin is filled in cation exchange column using wet method, at room temperature, by fume desulfurizing agent regenerative process pair
Product mixed solution is by resin bed, the Na in the accessory substance mixed solution of fume desulfurizing agent regenerative process generation+With resin
On NH4 +Generation exchange reaction, collects post bottom efflux, with the Na in efflux+Concentration reaches 5mg/L to collect terminal；Will
After the efflux of collection is acidified to pH value for 4~5 and drying through persulfuric acid, ammonium sulfate is obtained, complete to isolate and purify；
The NH4 +Type cationic ion-exchange resin is containing sulfonic resin；
By the NH after failure4 +It is 7~9 that type cationic ion-exchange resin is first washed with deionized to efflux pH value, then uses carbonic acid
Hydrogen ammonium salt solution, ammonium chloride solution or ammonium sulfate drip washing resin, it is 7~9 to be finally washed with deionized to efflux pH value,
Obtain NH4 +Type cationic ion-exchange resin, NH4 +Type cationic ion-exchange resin can be reused；
The flow velocity that the fume desulfurizing agent regenerative process accessory substance mixed solution passes through resin bed is 2~8BV/h；
The molar concentration of the ammonium bicarbonate soln, ammonium chloride solution or ammonium sulfate is 1~2mol/L, and ammonium hydrogen carbonate is molten
The volume of liquid, ammonium chloride solution or ammonium sulfate is 3~5BV；
The flow velocity of the ammonium bicarbonate soln, ammonium chloride solution or ammonium sulfate is 1.5~2BV/h；
Described is gel-network precipitation method Seplite LSI-010, macroporous type cation exchange containing sulfonic resin
Resin A mberlite FPC22Na or Amberlite 252Na；
By the NH after failure4 +When type cationic ion-exchange resin is first washed with deionized, the flow velocity of deionized water used for 6~
8BV/h。
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