CN102824833A - Method for removing and recovering sulfur dioxide in gas by use of low-energy-consumption and regenerable absorbent - Google Patents
Method for removing and recovering sulfur dioxide in gas by use of low-energy-consumption and regenerable absorbent Download PDFInfo
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- CN102824833A CN102824833A CN2011101634814A CN201110163481A CN102824833A CN 102824833 A CN102824833 A CN 102824833A CN 2011101634814 A CN2011101634814 A CN 2011101634814A CN 201110163481 A CN201110163481 A CN 201110163481A CN 102824833 A CN102824833 A CN 102824833A
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Abstract
The invention relates to a method for removing and recovering sulfur dioxide (SO2) in gas by use of low-energy-consumption and regenerable absorbent. The method is characterized by utilizing an absorbent to contact sulfur dioxide-containing gas to remove sulfur dioxide, wherein the absorbent contains two or more of inorganic alkali, composite salt thereof or sulfite 10-50 wt%, antioxidant 0-0.2 wt%, and water; desorbing the sulfur dioxide-containing absorbent to obtain high-concentration sulfur dioxide gas and regenerated absorbent; and circulating the regenerated absorbent for removing sulfur dioxide in mixed gas. The inventive method can realize cyclic regeneration and utilization of absorbent; and has the advantages of no secondary pollution, low energy consumption and operation cost during utilization process.
Description
Technical field
The present invention relates to a kind of employing Regeneratable absorbent and from mist, remove and reclaim sulfur dioxide (SO
2) method.
Background technology
SO
2Be China's atmosphere pollution major pollutants, annual discharge capacity is more than 2,000 ten thousand tons, and its main source is a large amount of low concentration SO that the field produced such as metallurgy, thermoelectricity, thermoelectricity and chemical industry
2Flue gas is therefore to SO in the flue gas
2Improvement is to reduce SO
2The major measure of polluting.
In existing sulfur removal technology, utilize SO in the direct absorbing and removing flue gas of absorbent
2Be one of most effectual way, method commonly used at present is:
The calcium method that is the basis with lime, lime stone is the magnesium method on basis with magnesia, and the sodium method that is the basis with sodium carbonate, NaOH is with NH
3Be the ammonia process on basis, and the metal oxide method etc.In order to last method, though can remove the SO in the flue gas
2, but in use, raw materials used generally all the need earlier through hydration process, and desulfurization product need carry out the aeration oxidation processes for reaching discharge standard, causes problems such as equipment investment is big, operation and maintenance cost height; And existing method can only solve SO merely
2Air pollution problems inherent, absorbent can't be realized recycle, causes a large amount of wastings of resources, produced simultaneously desulfurizing byproduct added value is low, often is difficult for selling, and is general directly discarded, is prone to cause secondary pollution problems.Like the soda method, utilize NaOH to absorb SO
2Behind the gas, byproduct is a sodium sulfite, and is much lower than the NaOH price, and in the use, factory drops into huge.And in the calcium method, utilize calcium hydroxide or calcium carbonate to absorb SO
2, obtaining calcium sulfate, this method exists low, the easy obstruction of absorptivity, byproduct not to have market etc.In the magnesium method, after magnesium hydroxide absorbs SO2, generate accessory substance magnesium sulfite and magnesium bisulfite, be oxidized to behind the magnesium sulfate it directly discarded usually.
For the recycling of absorbent commonly used, there is not better method at present.Propose to adopt in (CN1481926A) like domestic patent " a kind of flue gas desulfurization by magnesia wet method and product reclaim new technology " and in the absorption tower, propose underflow; Generate magnesium sulfate technology through oxidation; Do not relate to improvement, cause the secondary pollution of the wasting of resources and accessory substance flue gas desulfurization absorption and regeneration of absorption solution technology.And patent " sulfur removal technology of using external regenerative cycle magnesium sulfate method flue gas or waste gas " (CN101607173A) in; Utilize magnesia and magnesium bisulfite to obtain magnesium sulfite and carry out flue gas desulfurization through outer loop regeneration; But the method still needs continuous supplemental magnesium, and the magnesium bisulfite amount that generates simultaneously can get more and more, and fails really to realize the recycle absorbent; And end product also has to abandon as solid waste, has the wasting of resources and secondary pollution problem equally.
And absorption SO provided by the invention
2Method in conjunction with the advantage of existing desulfur technology, has avoided in the present technology absorbent can't recycle, causes the wasting of resources and desulfurization product pollution problem, and saves desulfurization product oxidizing process in the former technology, has reduced equipment investment and operating cost.The absorbent that this method is used, absorbability is big, and energy consumption is low, and absorbent is stable and can recycle and can reclaim high concentration SO
2Gas does not produce solid waste, and cost of investment is low, has better solved existing SO
2Remove the shortcoming of technology.
Summary of the invention
The invention provides a kind of absorbent medium of utilizing from containing SO
2Absorb SO in the gas
2, and the method that absorbent regeneration is recycled, this method key step is:
(1) makes and contain SO
2Gas contacts with absorbent, from this mist, absorbs SO
2, obtain meeting SO
2The gas of emission concentration standard be combined with SO
2Absorbent.
Wherein, absorbent contains inorganic base and/or its double salt and/or sulphite and anti-oxidant.
Inorganic base in the absorbent meets molecular formula M (OH)
x, wherein M is a metallic element, x is the valence state of M.Said inorganic base can with SO
2Generate solubility or microsolubility sulphite, bisulfites.Particularly, said alkali can be, for example Mg (OH)
2, Al (OH)
3, Mn (OH)
2, Zn (OH)
2, Cu (OH)
2, Fe (OH)
2, Fe (OH)
3Deng; Double salt is mainly the sulfate and the sulfurous acid of above inorganic base, and for example: alkali formula magnesium sulfite, alkali magnesium sulfate, alkali formula zinc sulfite, alkali formula aluminium sulfite etc. are preferably the alkali acid sulphite; Sulphite is mainly the sulphite of contained metallic element in the above inorganic base, for example: MgSO
3, ZnSO
3, CuSO
3, Al
2(SO
3)
3Deng.The above various inorganic base, its double salt and sulphite are merely for example, are not limited only to above content but contained inorganic base, its double salt and sulphite comprise.
Contained inorganic base, its double salt and sulphite can be single components in the prescription, also can be the combinations of two or more composition.
The anti-oxidant that contains in the absorbent is aromatic amine, phenols, quinones, alcohols, ethers and derivative thereof, or sulphur and thiosulfate; Aromatic amine such as diphenylamines, p-phenylenediamine (PPD), EEDQ etc.; Phenols such as hydroquinones etc.; Quinones as: 2, the 6-tert-butyl group-4-methylphenol anthraquinone, 2-methylanthraquinone etc.; Alcohols is like ethanol, two 12 carbon alcohol esters, two ten four carbon alcohols esters and two octadecanol esters etc.; Ethers such as MEHQ, two (3, three grades of butyl of 5--4-hydroxy phenyl) thioether glycol ether etc.; Thiosulfate is like sodium thiosulfate, magnesium thiosulfate etc.; Be preferably benzenediol, 2-methylanthraquinone, MEHQ, thiosulfate etc.Its effect is to prevent that absorbent from absorbing SO
2After the sulphite and the bisulfites that obtain be stable sulfate by the dioxygen oxidation in the gas, hinder the regeneration of absorbent.The above various anti-oxidant is merely for example; Those skilled in the art should know; All can prevent the material of sulphite and bisulfites oxidation, all can be used as the anti-oxidant among the present invention, and the used anti-oxidant of the present invention includes but are not limited to above content.
Contained anti-oxidant can be single component in the prescription, also can be the combination of two or more anti-oxidant.
Also contain water in the absorbent.
Particularly, absorbent contains: the inorganic base of 10%~50% quality, its double salt and sulphite or both and both above mixtures are preferably 10%~30% quality; The anti-oxidant of 0~0.2% quality is preferably 0.05~0.15% quality; Solvent is a water; Each component sum is 100% quality.
Step (1) is preferably carried out under 10~70 ℃ of temperature, is preferably 20~60 ℃.
In the step (1), absorbent and SO
2Mass ratio be that 200~500g absorbent absorbs 100g SO
2Quality, be preferably 200~400g absorbent and absorb 100g SO
2Quality.
SO
2Emission concentration standard is the corresponding discharge standard of every profession and trade that meets the provisions of the relevant regulations issued by the State.
Absorbent absorbs SO
2After, along with SO in the absorbent
2The increase of content, the pH value can decrease, to SO
2Therefore absorption efficiency also can decrease, and what generate is combined with SO
2Absorbent final pH value is preferably 4.0~5.5 between 2.0~6.0, control final absorbent pH value through regulating the absorber portion liquid-gas ratio.
Be combined with SO
2The absorbent main component be that contained inorganic base in the absorbent, its double salt and sulphite absorb SO
2After the sulfate mixture that obtains of the sulphite, bisulfites and the oxidation thereof that are converted into, wherein be main component with the bisulfites.The mechanism reaction equation is following:
SO
2+H
2O→H
2SO
3 (1-1)
H
2SO
3→H
++HSO
3 - (1-1)
M(SO
3)
x/2+x/4O
2→M(SO
4)
x/2 (1-5)
M(HSO
3)
x+x/2O
2→M(SO
4)
x/2+x/2H
2SO
4 (1-6)
yM(SO
3)
x/2·M(OH)
x+x/2SO
2→(y+1)M(SO
3)
x/2+x/2H
2O (1-7)
(2) to obtaining being combined with SO
2Absorbent carry out desorb, with gaseous state SO
2From absorbent, separate sucking-off, obtain high-purity SO
2Gas and absorbent regeneration.
Desorption process steam stripped capable of using, or pass the absorbent stripping, or through the thin film evaporator desorb through inert gas, or carry out through methods such as atomization and vaporization desorbs, temperature is controlled at 20~110 ℃, is preferably 70~105 ℃; Above method can also can be carried out under negative pressure at normal pressure, and the unstable salt in the solution is decomposed, and separates sucking-off SO
2Gas.
M(HSO
3)
x→M(SO
3)
x/2+x/2SO
2↑+x/2H
2O (2-1)
(a+b)M(SO
3)
x/2·cH
2O→aM(SO
3)
x/2·bM(OH)
x+bx/2SO
2↑+(c-bx/2)H
2O (2-2)
In the desorption process, SO thereupon
2Separate out, the pH value of absorbent raises usually, along with the pH value raises, and SO
2The difficulty of desorb also increases, and the pH value of the absorbent regeneration that obtains after the desorb is preferably 6.0~7.5 between 5.5~9.5.
Main component is the sulphite and the double salt thereof of contained metallic element in inorganic base, its double salt and the sulphite that is contained in the former absorbent in the absorbent regeneration, and contains the small amount of sulfur hydrochlorate.
(3) detect sulphates content in this absorbent regeneration,, sulfate is separated from absorbent regeneration, guarantee that absorbent regeneration is to SO when surpassing when allowing content
2Adsorption capacity.
Sulfate in the absorbent regeneration is to be generated by dioxygen oxidation sulphite in the mist and bisulfites.Reaction mechanism is shown in reaction equation (1-5), (1-6).
For making absorbent regeneration more effectively absorb SO
2, the permission content of sulfate should be controlled at below the 10 quality %, is preferably below the 5 quality %.
The removal method of sulfate ion can be according to the different physicochemical characteristics with sulphite of sulfate, as: methods such as difference in solubility are removed; Or the employing electrochemical method, as: methods such as electrodialysis are carried out separating cycle regeneration with sulfate in the absorbent regeneration and sulphite; Or adopt method such as anion exchange resin to remove.
(4) because in desorption process; Certain water loss is arranged; Therefore contained sulfurous acid and double salt amount concentration thereof are higher in the absorbent regeneration that obtains; Need to replenish a certain amount of moisture content, make in the absorbent regeneration sulphite and double salt total amount thereof remain on 10~50 quality %, then this absorbent regeneration is got back to recycle in the step (1).
Compared with prior art, adopt method of the present invention to absorb SO
2, to invest lowly, operating cost is low in the use, and energy consumption is low, non-secondary pollution.
Method of the present invention and MgO method compare, and desulfurization product is aerobicization not, reduced equipment investment, and in absorption process, single with Mg (OH)
2Be absorbent, but be absorbent with inorganic base and double salt thereof or two kinds of mixtures.In the method for the invention, inorganic base and double salt thereof or two kinds of mixtures absorb SO
2The back generates M (SO
3)
X/2And M (HSO
3)
x,, obtain high concentration SO through this solution is carried out desorb
2And absorbent regeneration, directly circulation is used to absorb SO
2, realize the circular regeneration of absorbent, and temperature being 20~110 ℃ during regeneration, energy consumption is lower.And in the existing MgO technology, general with the MgSO that obtains
3Product is oxidized to MgSO
4, MgSO
4Added value is lower, and is general directly discarded, forms secondary pollution easily; Perhaps with MgSO
3And Mg (HSO
3)
2Heat to decompose more than 800 ℃ and obtain the MgO that regenerates, the realization absorbent regeneration.Compare with this method, the absorbent regeneration energy consumption is bigger, and when high temperature regeneration, part MgO meeting inactivation causes the absorbent loss.
Description of drawings
Accompanying drawing 1 process of desulfurizing gases simplified flow chart of the present invention
Specific embodiment
The present invention will be described below in conjunction with instance, but its purpose is not a restriction range of application of the present invention.
Embodiment 1
A certain 20t/h chain furnace boiler exhaust gas, SO in the gas
2Content is 2000~5000ppm, and temperature is 150 ℃.After wherein drawing part of smoke entering absorption tower, through spray washing, remove wherein dust and SO earlier
3And cooling, get into absorber portion then, under 60~70 ℃ of temperature, through spray absorbent is contacted with flue gas, the SO in the flue gas
2Be absorbed agent and absorb, gas is discharged from the top, absorption tower, absorbs SO
2The pH value that the back absorbs the back agent is 4.5~5.0, then gets in the steam desorber, obtains SO through the low-pressure steam desorb
2Gas and pH value are 5.6~5.8 absorbent regenerations.Detect sulphates content in the absorbent regeneration, when contained sulfate surpasses regulation 10%, sulfate ion is removed through anion-exchange resin method.Replenish certain water gaging in the absorbent regeneration, making the mass concentration of active ingredients such as wherein contained sulphite and double salt thereof is 35~40%, then this absorbent regeneration is sent into recycle in the absorption tower.
Absorbent component is: the Mg of 20 quality % (OH)
2, 0.2 quality % magnesium thiosulfate, all the other are water;
Its service data is following:
Embodiment 2
Like condition among the embodiment 1, difference is:
Absorbent component is: 10 quality %Mg (OH)
2, 5 quality % alkali formula magnesium sulfites, 5 quality % magnesium sulfites, 0.1 quality % sulphur, all the other are water;
Absorb SO
2Back absorbent pH value is 4.0~4.5;
Desorption apparatus adopts low pressure spraying desorb, and pressure is-0.05MPa that temperature is 80 ℃, obtains SO
2Gas and absorbent regeneration, absorbent regeneration pH value is 5.8~6.0, makes through anion exchange resin that the magnesium sulfate mass concentration is lower than 10% in the reproducing adsorbent.
The mass concentration that finally enters into the active ingredient such as absorbent regeneration magnesium sulfite and double salt thereof of absorption tower recycle is 35~40%.
Its service data is following:
Embodiment 3
Like condition among the embodiment 1, difference is:
Absorbent component is: 15 quality %Al (OH)
3, 0.1 quality % p-phenylenediamine (PPD), 0.05 quality % ethanol, all the other are water;
Absorb SO
2The pH value of back absorbent is 3.5~4.0;
Absorbent regeneration pH value is 6.0~6.2, and the aluminum sulfate mass concentration should be lower than 10%, and the mass concentration that finally enters into simultaneously the active ingredients such as absorbent regeneration aluminium sulfite and double salt thereof of absorption tower recycle is 25~30%.
Its service data is following:
Embodiment 4
Like condition among the embodiment 1, difference is:
Absorbent component is: 15 quality %Mn (OH)
2, 0.1 quality % hydroquinones, all the other are water;
Absorb SO
2The pH value of back absorbent is 4.0~4.5;
Absorbent regeneration pH value is 6.0~6.2;
The manganese sulfate mass concentration should be lower than 10% in the absorbent regeneration, and the mass concentration that finally enters into simultaneously the active ingredients such as absorbent regeneration manganous sulfite and double salt thereof of absorption tower recycle is 30~35%.
Its service data is following:
Embodiment 5
Like condition among the embodiment 1, difference is:
Absorbent component is: 18%Zn (OH)
2, 0.1 quality %2-tectoquinone, all the other are water;
Absorb SO
2The pH value of back absorbent is 4.0~4.5;
In conjunction with SO
2Absorbent adopts the low pressure atomization method to carry out desorb, after desorb, obtains SO
2Gas and absorbent regeneration, absorbent regeneration control pH value is 5.8~6.0.
In the absorbent regeneration, the zinc sulfate mass concentration should be lower than 8%, and the mass concentration that finally enters into simultaneously the active ingredients such as absorbent regeneration zinc sulfite and double salt thereof of absorption tower recycle is 25~30%.
Its service data is following:
Embodiment 6
A certain smeltery sinter fume, SO in the gas
2Content is 7000~13000ppm, and temperature is 50~60 ℃.After flue gas gets into the absorption tower, the SO in the flue gas
2Be absorbed agent and absorb, gas is discharged from the top, absorption tower, absorbs SO
2Back absorbent pH value is 3.5~4.0, and then absorbent is introduced in the thin film evaporator, carries out gas and carries, and obtains SO
2Gas and absorbent regeneration, reproducibility absorbent pH value is 6.0~6.5.
Detect sulphates content in the absorbent regeneration, when contained sulfate surpasses regulation 10%, sulfate ion is removed through electroosmose process.Add a certain amount of water in the absorbent regeneration, making the mass concentration of active ingredients such as wherein contained sulphite and double salt thereof is 40~45%, then this absorbent regeneration is sent into recycle in the absorption tower.
Absorbent component is: 30 quality % alkali formula magnesium sulfites, and two (3, three grades of butyl of 5--4-hydroxy phenyl) the thioether glycol ethers of 0.1 quality %, all the other are water;
Its service data is following:
Embodiment 7
Like condition among the embodiment 6, difference is:
Absorbent component is: 25 quality %Cu (OH)
2, 5 quality % alkali formula sulfurous acid copper, 0.1 quality % MEHQ, all the other are water;
Absorb SO
2Back absorbent pH value is 4.0~4.5;
Absorbent regeneration control pH value is 6.2~6.5;
In the absorbent regeneration, the copper sulphate mass concentration should be lower than 10%, and the mass concentration that finally enters into simultaneously the active ingredients such as absorbent regeneration Central Asia copper sulphate and double salt thereof of absorption tower recycle is 45~50%.
Its service data is following:
Embodiment 8
Like condition among the embodiment 6, difference is:
Absorbent component is: 15 quality %Fe (OH)
2, 10 quality %Fe (OH)
3, 0.1 quality % sodium thiosulfate, the two 12 carbon alcohol esters of 0.05% quality %, all the other are water;
Absorb SO
2Back absorbent pH value is 4.5~4.8;
Absorbent regeneration control pH value is 5.8~6.0;
In the absorbent regeneration, ferric sulfate and ferrous sulfate mass concentration should be lower than 10%, and the mass concentration that finally enters into the active ingredients such as absorbent regeneration Central Asia ferric sulfate, ferrous sulfite and double salt thereof of absorption tower recycle simultaneously is 45~50%.
Its service data is following:
Claims (11)
1. one kind is utilized absorbent from containing SO
2Absorb SO in the mist
2And make the method for absorbent circular regeneration through processing, comprise the steps:
(1) makes and contain SO
2Gas contacts with absorbent, absorbs the SO in this gas
2, formation meets SO
2The gas of emission concentration standard be combined with SO
2Absorbent;
(2) SO that is combined with to obtaining
2Absorbent carry out desorb, collect SO
2Gas obtains absorbent regeneration simultaneously, and wherein said absorbent regeneration is back in the step (1);
It is characterized in that: said absorbent contains inorganic base and/or its double salt and/or sulphite and anti-oxidant.
2. the method described in claim 1, wherein the described inorganic base of absorbent meets molecular formula: M (OH)
x, wherein M is a metallic element, x is the valence state of M.
3. according to claim 1 or claim 2 method, wherein the inorganic base in the absorbent is Mg (OH)
2, Al (OH)
3, Mn (OH)
2, Zn (OH)
2, Cu (OH)
2, Fe (OH)
2And/or Fe (OH)
3Said double salt is the sulfate and the sulphite of said inorganic base; Said sulphite is the sulphite of contained metallic element in the said inorganic base.
4. like each described method in the claim 1 ~ 3; Wherein the composition of absorbent is: the inorganic base of 10% ~ 50% quality, its double salt and sulphite or both and both above mixtures; 0.0 the anti-oxidant of ~ 0.2% quality, and water, each component sum are 100 % quality.
5. like each described method in the claim 1 ~ 4, wherein, anti-oxidant is aromatic amine, phenols, quinones, alcohols, ethers and derivative thereof, sulphur or thiosulfate in the absorbent.
6. according to the method described in the claim 1, what generate in the step (1) is combined with SO
2Absorbent contain by inorganic base, its double salt and sulphite and absorb SO
2After the sulfate mixture that obtains of the sulphite, bisulfites and the oxidation thereof that are converted into.
7. the method for claim 1 is characterized in that: in step (1), control and be combined with SO
2Absorbent final pH value is 2.0 ~ 6.0, is preferably 4.0 ~ 5.5.
8. the method for claim 1, it is characterized in that: in step (2), the pH value of the absorbent regeneration that obtains after the desorb is 5.5 ~ 9.5, is preferably 6.0 ~ 7.5.
9. the method for claim 1 is included in step (2) absorbent regeneration reuse afterwards step (3) before: detect the sulphates content in this absorbent regeneration, will exceed permission content sulfate and from absorbent regeneration, separate.
10. method as claimed in claim 9 is included in step (3) absorbent regeneration reuse afterwards step (4) before: with the absorbent regeneration supplementing water, regulate the concentration of absorbent, be recycling it to the SO that absorbs in (1) in the gas
2
11. method as claimed in claim 9 is characterized in that: in step (3), sulphates content is controlled at below 10% quality in the absorbent regeneration, is preferably below 5% quality.
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