CN102872718B - Oxidation method of wet flue gas desulfurizing liquid - Google Patents
Oxidation method of wet flue gas desulfurizing liquid Download PDFInfo
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- CN102872718B CN102872718B CN201110192783.4A CN201110192783A CN102872718B CN 102872718 B CN102872718 B CN 102872718B CN 201110192783 A CN201110192783 A CN 201110192783A CN 102872718 B CN102872718 B CN 102872718B
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- doctor solution
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Abstract
The invention discloses a catalytic oxidation method of a wet flue gas desulfurizing liquid. According to the method, a SO2 absorbed desulfurizing liquid and air continuously pass through a fixed bed reactor filled with a catalyst and react in the presence of the honeycomb ceramic catalyst and under a proper oxidation condition, wherein the catalyst is a honeycomb ceramic catalyst and an active metal component is rare-earth oxide. By the adoption of the method, oxidation rate and oxygenation efficiency of sulfite are significantly raised. During the application of the catalyst, there is no loss of active components. Therefore, operation cost is reduced, and secondary pollution caused by loss of active components is also effectively avoided. In addition, the honeycomb ceramic catalyst used also has advantages of high mechanical strength, wear resistance, little fluid resistance, long service life and the like. The method provided by the invention provides an effective processing method for the discharge of the wet flue gas desulfurizing liquid to reach the standard.
Description
Technical field
The present invention relates to the oxidation technology of wet process of FGD liquid, the catalytic oxidation technologies especially relating to wet process of FGD liquid sulfite salt and the catalyst used thereof.
Background technology
During combustion of sulfurous fuel, except a part of sulphur is contained in except in cigarette ash, other parts will be thrown into air in the form of sulphur dioxide.Sulfur dioxide not only works the mischief to health, but also can form acid rain, causes serious pollution to environment.Therefore, large-scale burner generally all equips flue gas desulfur device, and wherein majority is wet flue gas desulfurizer.
Main containing sulphite in the doctor solution obtained after usual wet desulphurization, for the ease of sulphite utilization and make the wastewater to reach standard of discharge, needing sulfite oxidation is sulfate.Industrial being typically employed at the bottom of absorption tower arranges storage tank, and the doctor solution stored in storage tank passes into air with the form of bubbling, oxidative salt.But this mode oxidation rate is very slow, probably need 4 ~ 5 hours as calcium sulfite transforms 90%; Magnesium sulfite transforms 90% needs 7 ~ 8 hours.Therefore, desulfurization product usually reaches capacity very soon because oxidation rate is slow and precipitates in absorbing liquid.In addition, the COD of efflux wastewater is also usually higher than national standard.
CN101259366A discloses a kind of method for oxidation in flue gas desulfurization course.Promote that doctor solution sulfite salt is oxidized to sulfate by three kinds of modes: one is pass into air directly in flue gas; Two is separately establish an air delivery pipe in absorption equipment, and air is sent into and mixed in absorption tower with flue gas; Three be at gas and liquid flowing under when, pass into air in " slurries " agent exit, by arrange Liqiud-gas mixing device, make air and " slurries " mixing.
CN1565709A discloses a kind of catalytic oxidation technique of flue gas desulfurization product, at flue gas SO
2add appropriate soluble salts catalyst in absorbing liquid, when containing 0.001 ~ 0.02mol/L catalyst in absorbing liquid, desulfurization product reaches more than 90.6% at the conversion ratio of 2 hours.CN101244360A discloses a kind of catalytic oxidation technique of calcium sulfite, and this technique is at absorption SO
2after slurries in add soluble ferric iron salt, manganese salt or the mixture of both as catalyst.Above two kinds of patents all adopt soluble-salt to be converted into sulfate as catalyst sulphite, soluble-salt inevitably runs off in application process, therefore need constantly to supplement soluble-salt, not only running cost is high, and soluble-salt also can cause the secondary pollution of doctor solution.
CN101219340A discloses a kind for the treatment of process of discharged doctor solution of HPF desulfurization system of coke-oven plant.The method comprises following operation: A. catalytic oxidation-selection complexing; B. press filtration or centrifugation; C. product generates; D. complexing agent regeneration.Add complexing agent in this treatment process and be used as oxidation catalyst, running cost is high.
Summary of the invention
For the deficiencies in the prior art, the invention provides oxidation technology and the catalyst of the doctor solution after a kind of smoke-gas wet desulfurization, this technique is simple, and operating cost is low, non-secondary pollution, the oxidation of catalyst to the sulphite in doctor solution has good catalytic activity and stability.
A catalysed oxidation processes for flue gas desulfurization liquid, is characterized in that making absorption SO
2after doctor solution and air enter the fixed bed reactors that catalyst is housed continuously, carry out oxidation reaction in the presence of an oxidation catalyst.
According to catalysed oxidation processes of the present invention, described doctor solution and oxygen can pass through fixed bed reactors in the mode also flowed.As described in doctor solution and air enter reactor from the top of reactor, to exist and under suitable oxidizing condition, with downflow system by fixed bed reactors, reaction afterproduct leaves reactor from reactor bottom at catalyst; Or doctor solution and air enter reactor from reactor bottom, under catalyst existence and suitable oxidizing condition, in upper reaches mode by fixed bed reactors, reacted product leaves reactor from reactor top.
According to catalysed oxidation processes of the present invention, described course of reaction can be counter-current modes of operation: doctor solution enters reactor from reactor head, oxygen enters reactor from reactor bottom, under the existence and suitable oxidizing condition of catalyst, passes through fixed bed reactors in a counter-current fashion.
The operating condition of doctor solution oxidation reaction is: doctor solution volume space velocity is 0.1 ~ 10h
-1, preferably 0.5 ~ 5h
-1; Air/doctor solution volume ratio is 5 ~ 200, preferably 10 ~ 100; In the inventive method, reaction temperature and pressure do not need to control, by the doctor solution temperature and pressure discharged during flue gas desulfurization normal operating.
Wherein said absorption SO
2the composition of doctor solution different according to the difference of absorbent in flue gas desulfurization course.One or more in sodium sulfite, magnesium sulfite and calcium sulfite are generally comprised in doctor solution.The concentration of doctor solution sulfite salt is 0.1g/L ~ 100g/L, and doctor solution pH value is 4 ~ 8.
Wherein said oxidation catalyst is honeycomb ceramic type catalyst, this catalyst matrix is ceramic honey comb, coated carrier is selected from one group of material of aluminium oxide, zirconia, titanium oxide composition, and active metal component is selected from one or more in lanthana, cerium oxide, praseodymium oxide, neodymia and samarium oxide.With the weight of catalyst for benchmark, coated carrier proportion is 5 ~ 30%, and the content of active metal component counts 1% ~ 10% with metal.
Described honeycomb ceramic type catalyst can adopt the preparation of following method: first ceramic honey comb matrix impregnates is contained aluminium oxide, zirconia, titanium oxide or wherein two or three the slurries of composite oxides, take out, blow away unnecessary slurries in duct, drying and roasting obtain the ceramic honey comb of coated carrier coating; Next by the salting liquid of the ceramic honey comb dipping rare earth metal of coating good vector coating, take out, blow away unnecessary slurries in duct, drying and roasting can prepare this catalyst.
Compared with prior art, the method for oxidation tool of smoke-gas wet desulfurization liquid of the present invention has the following advantages:
1, this method improves the oxidation rate of sulphite, effectively reduces sulphite in intrasystem deposition.When especially adopting magnesium processes desulfurization, because the solubility of magnesium sulfite is very little, the oxidation rate of existing technique sulfite magnesium is slow, usually causes sediment to occur; After adopting this technique, the oxidation rate of magnesium sulfite improves greatly, and the solubility of oxidation product magnesium sulfate, much larger than magnesium sulfite, avoids the appearance of sediment.
2, this method improves the oxygenation efficiency of sulphite, and makes the COD of desulfurization efflux wastewater up to standard.For the desulfurization of employing calcium method, adopt this technique to improve the purity of oxidation product gypsum, gypsum is had a good application prospect.
3, the inventive method adopts rare-earth metal catalyst as oxidation catalyst.It has been generally acknowledged that, rare-earth oxide has good carrier property and stability, and it is typically used as catalyst carrier, as Fe
2o
3/ CeO
2catalyst.And in the inventive method, applicant surprisingly finds, adopt rare-earth oxide as catalyst activity metal component, gained catalyst has good catalytic oxidation performance equally, can meet the needs of doctor solution sulfite salt oxidation completely.Particularly valuable, the loss of rare-earth metal catalyst in use inactive component, can reuse, thus reduce running cost, also effectively can avoid the secondary pollution caused because active metal component runs off.And in prior art, as adopted soluble manganese salt as catalyst oxidation sweetening liquid in patent CN1565709A, the concentration of described soluble manganese salt in doctor solution is at more than 0.001mol/L.After doctor solution oxidation, the manganese contained in doctor solution is up to more than 275mg/L, total manganese discharge standard (<5mg/L) of regulation in country's " sewage drainage standard ", bring new secondary pollution, need subsequent process to reclaim or remove the manganese in doctor solution, complex treatment process, operating cost is high.
4, to be that ceramic honeycomb catalyst has mechanical strength high, wear-resistant for solid catalyst of the present invention, the advantages such as fluid resistance is little, and the life-span is long.
Detailed description of the invention
The specific embodiment of the present invention carries out exemplary explanation in more detail by by following examples, and described embodiment should not be construed as the restriction of the scope of the invention.
ZrO in embodiment
2, TiO
2be commercially available prod with boehmite, cerous nitrate used, lanthanum nitrate, samaric nitrate etc. are chemically pure reagent.
Embodiment 1
The preparation of doctor solution oxidation catalyst:
(1) preparation of coating slurry
By 20 grams of ZrO
2, 20 grams of TiO
2add 240 ml deionized water and stirring after mixing with 8 grams of boehmites, above-mentioned mixed serum is placed in ball mill ball milling and namely obtains required coating slurry.
(2) coating slurry coating
In the coating slurry configured in step (1) by 63.15 grams of cordierite honeycomb ceramic matrix impregnates, blow away the raffinate in duct after taking-up, 100 DEG C of dryings 5 hours, 500 DEG C of roastings 5 hours.
(3) load of active component
Take 18 grams of cerous nitrates and 28 grams of lanthanum nitrates are dissolved in 500ml deionized water, the sample having applied coating in step (2) is flooded in above-mentioned solution, take out, blow away raffinate, 100 DEG C of dryings 2 hours, 500 DEG C of roastings 5 hours, can obtain this honeycomb fashion doctor solution oxidation catalyst.Catalyst is expressed as CeLa/TiO
2-ZrO
2-Al
2o
3/ CH, wherein coated carrier TiO
2-ZrO
2-Al
2o
3proportion is 10wt%, active component CeLa content be 5wt%, Ce/La is 1:2.
Doctor solution is oxidized:
Doctor solution sulfite na concn is 2200 mg/L, COD is 432 mg/L, and pH value is 7.1, and doctor solution enters fixed bed reactors from reactor head, and air enters fixed bed reactors and doctor solution counter current contacting, at CeLa/TiO from reactor bottom
2-ZrO
2-Al
2o
3react under the catalytic action of/CH catalyst (catalyst volume 100mL).Reaction condition is: doctor solution volume space velocity is 3 h
-1, reaction temperature is 45 DEG C, and air/doctor solution volume ratio is 200.After question response stablizes 60 minutes, sample analysis ion concentration of inferior sulfate radical and COD.
Embodiment 2
Ce/ZrO is prepared according to the preparation method of embodiment 1
2/ CH, wherein coated carrier ZrO
2proportion is 5 wt%, active component Ce content is 1 wt% catalyst.
Doctor solution is oxidized:
Doctor solution sulfite na concn is 2670 mg/L, COD is 512 mg/L, and pH value is 7.2, and doctor solution enters fixed bed reactors from reactor head, and air enters fixed bed reactors and doctor solution counter current contacting, at Ce/ZrO from reactor bottom
2react under the catalytic action of/CH catalyst (catalyst volume 100mL).Reaction condition is: doctor solution volume space velocity is 4 h
-1, reaction temperature is 54 DEG C, and air/doctor solution volume ratio is 100.After question response stablizes 60 minutes, sample analysis ion concentration of inferior sulfate radical and COD.
Embodiment 3
Pr/ZrO is prepared according to the preparation method of embodiment 1
2/ CH, wherein coated carrier ZrO
2proportion is 10 wt%, active component Pr content is 3 wt% catalyst.
Doctor solution is oxidized:
Doctor solution sulfite na concn is 2860 mg/L, COD is 548 mg/L, and pH value is 7.3, and doctor solution enters fixed bed reactors from reactor head, and air enters fixed bed reactors and doctor solution counter current contacting, at Pr/ZrO from reactor bottom
2react under the catalytic action of/CH catalyst (catalyst volume 100mL).Reaction condition is: doctor solution volume space velocity is 1h
-1, reaction temperature is 55 DEG C, and air/doctor solution volume ratio is 10.After question response stablizes 60 minutes, sample analysis ion concentration of inferior sulfate radical and COD.
Embodiment 4
Adopt CeLa/TiO prepared by embodiment 1
2-ZrO
2-Al
2o
3/ CH catalyst.
Doctor solution is oxidized:
Doctor solution sulfite na concn is 4311 mg/L, COD is 710 mg/L, and pH value is 7.5, and doctor solution and air enter fixed bed reactors from reactor head, at CeLa/TiO
2-ZrO
2-Al
2o
3under the existence of/CH catalyst (catalyst volume 100mL), and stream passes downwardly through fixed bed reactors.Reaction condition is: doctor solution volume space velocity is 0.5h
-1, reaction temperature is 50 DEG C, and air/doctor solution volume ratio is 80.After question response stablizes 60 minutes, sample analysis ion concentration of inferior sulfate radical and COD.
Embodiment 5
Adopt CeLa/TiO prepared by embodiment 1
2-ZrO
2-Al
2o
3/ CH catalyst.
Doctor solution is oxidized:
Doctor solution sulfite magnesium density is 3132 mg/L, COD is 588 mg/L, and pH value is 7.4.Doctor solution and air enter fixed bed reactors from reactor bottom, at CeLa/TiO
2-ZrO
2-Al
2o
3under the existence of/CH catalyst (catalyst volume 100mL), and pass through fixed bed reactors on flowing to.Reaction condition is: doctor solution volume space velocity is 1.8h
-1, reaction temperature is 48 DEG C, and air/doctor solution volume ratio is 20.After question response stablizes 60 minutes, sample analysis ion concentration of inferior sulfate radical and COD.
Embodiment 6
The preparation of catalyst: prepare Sm/TiO according to the preparation method of embodiment 1
2-ZrO
2/ CH, wherein coated carrier TiO
2-ZrO
2proportion is 15wt%, active component Sm content is 8wt%.
Doctor solution is oxidized:
Doctor solution sulfite calcium concentration is 145 mg/L, COD is 95 mg/L, and pH value is 4.5.Doctor solution and air enter fixed bed reactors from reactor bottom, at Sm/TiO
2-ZrO
2under the existence of/CH catalyst (catalyst volume 100mL), and pass through fixed bed reactors on flowing to.Reaction condition is: doctor solution volume space velocity is 1.8h
-1, reaction temperature is 40 DEG C, and air/doctor solution volume ratio is 200.
Embodiment 7
Nd/TiO is prepared according to the preparation method of embodiment 1
2/ CH catalyst, wherein coated carrier TiO
2proportion is 30 wt%, active component Nd content is 10 wt%.
Doctor solution is oxidized:
Doctor solution sulfite na concn is 92000 mg/L, COD is 18900 mg/L, and pH value is 7.9.Doctor solution and air enter fixed bed reactors from reactor bottom, at Nd/TiO
2under the existence of/CH catalyst (catalyst volume 100mL), and pass through fixed bed reactors on flowing to.Reaction condition is: doctor solution volume space velocity is 0.1h
-1, reaction temperature is 65 DEG C, and air/doctor solution volume ratio is 150.After question response stablizes 60 minutes, sample analysis ion concentration of inferior sulfate radical and COD.
Embodiment 8
Ce/ZrO is prepared according to the preparation method of embodiment 1
2-Al
2o
3/ CH catalyst, wherein coated carrier ZrO
2-Al
2o
3proportion is 20 wt%, active component Ce content is 5 wt%.
Doctor solution is oxidized:
Doctor solution sulfite na concn is 80000 mg/L, COD is 16500 mg/L, and pH value is 7.6.Doctor solution and air enter fixed bed reactors Ce/ZrO from reactor bottom
2-Al
2o
3under the existence of/CH catalyst (catalyst volume 100mL), and pass through fixed bed reactors on flowing to.Reaction condition is: doctor solution volume space velocity is 2 h
-1, reaction temperature is 50 DEG C, and air/doctor solution volume ratio is 80.After question response stablizes 60 minutes, sample analysis ion concentration of inferior sulfate radical and COD.
Embodiment 9
CeSm/Al is prepared according to the preparation method of embodiment 1
2o
3/ CH catalyst, wherein coated carrier Al
2o
3proportion is 12 wt%, active component CeSm content be 1 wt%, Ce/Sm is 2:1.
Doctor solution is oxidized:
Doctor solution sulfite na concn is 1200 mg/L, COD is 320 mg/L, and pH value is 5.6.Doctor solution and air enter fixed bed reactors from reactor bottom, CeSm/Al
2o
3under the existence of/CH catalyst (catalyst volume 100mL), and pass through fixed bed reactors on flowing to.Reaction condition is: doctor solution volume space velocity is 5 h
-1, reaction temperature is 55 DEG C, and air/doctor solution volume ratio is 50.After question response stablizes 60 minutes, sample analysis ion concentration of inferior sulfate radical and COD.
Comparative example 1
Except not adding catalyst, the other the same as in Example 1.
Comparative example 2
Doctor solution composition is identical with embodiment 3.MnSO is added in doctor solution
4, as the Mn added
2+when reaching 0.005mol/L, the indexs such as the oxygenation efficiency of the sulphite that reactor outlet records and COD are just suitable with embodiment 3, but containing concentration in the doctor solution after oxidation is the Mn of 275mg/L, total manganese discharge standard (<5mg/L) of regulation in country's " sewage drainage standard ", bring new secondary pollution, need subsequent process to reclaim or remove the manganese in doctor solution, make its treatment process more complicated, operating cost is high.
Reaction result is in table 1.
The oxidation results of table 1 sulphite
| Embodiment and comparative example | Sulfite oxidation rate, % | COD，mg/L |
| Embodiment 1 | 98.5 | 74 |
| Comparative example 1 | 63.2 | 168 |
| Embodiment 2 | 99.1 | 66 |
| Embodiment 3 | 99.4 | 57 |
| Embodiment 4 | 99.1 | 68 |
| Embodiment 5 | 99.1 | 75 |
| Embodiment 6 | 98.6 | 57 |
| Embodiment 7 | 99.8 | 64 |
| Embodiment 8 | 99.4 | 67 |
| Embodiment 9 | 99.3 | 33 |
Claims (7)
1. a flue gas desulfurization liquid catalysed oxidation processes, is characterized in that, makes absorption SO
2after doctor solution and air enter the fixed bed reactors that catalyst is housed continuously, carry out oxidation reaction in the presence of an oxidation catalyst, the operating condition of doctor solution oxidation reaction is: doctor solution volume space velocity is 0.1 ~ 10h
-1, air/doctor solution volume ratio is 5 ~ 200; Wherein,
Described doctor solution comprises one or more in sodium sulfite, magnesium sulfite and calcium sulfite, and the concentration of doctor solution sulfite salt is 0.1g/L ~ 100g/L, and doctor solution pH value is 4 ~ 8;
Described oxidation catalyst is honeycomb ceramic type catalyst, this catalyst matrix is ceramic honey comb, coated carrier is selected from one group of material of aluminium oxide, zirconia, titanium oxide composition, and active metal component is selected from one or more in lanthana, cerium oxide, praseodymium oxide, neodymia and samarium oxide.
2. according to catalysed oxidation processes according to claim 1, it is characterized in that, described doctor solution and oxygen pass through fixed bed reactors in the mode also flowed.
3. according to catalysed oxidation processes according to claim 2, it is characterized in that, described doctor solution and air enter reactor from the top of reactor, under catalyst existence and suitable oxidizing condition, with downflow system by fixed bed reactors, reaction afterproduct leaves reactor from reactor bottom.
4. according to catalysed oxidation processes according to claim 2, it is characterized in that, described doctor solution and air enter reactor from reactor bottom, under catalyst existence and suitable oxidizing condition, in upper reaches mode by fixed bed reactors, reacted product leaves reactor from reactor top.
5. according to catalysed oxidation processes according to claim 1, it is characterized in that, described doctor solution enters reactor from reactor head, and oxygen enters reactor from reactor bottom, under the existence and suitable oxidizing condition of catalyst, pass through fixed bed reactors in a counter-current fashion.
6. according to catalysed oxidation processes according to claim 1, it is characterized in that, the operating condition of doctor solution oxidation reaction is: doctor solution volume space velocity is 0.5 ~ 5h
-1; Air/doctor solution volume ratio is 10 ~ 100.
7. according to catalysed oxidation processes according to claim 1, it is characterized in that, with the weight of catalyst for benchmark, coated carrier proportion is 5 ~ 30%, and the content of active metal component counts 1% ~ 10% with metal.
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| CN106745155B (en) * | 2016-11-29 | 2018-10-23 | 安徽工业大学 | A kind of flue gas desulfurization byproduct modification processing method |
| CN106823750A (en) * | 2017-03-24 | 2017-06-13 | 华北电力大学（保定） | It is a kind of to be aoxidized for magnesium processes desulfurization sulfite salt and the device for cooperateing with demercuration |
| CN111389467B (en) * | 2020-03-19 | 2022-05-24 | 河北中垒新能源科技有限公司 | Limestone-gypsum wet desulphurization catalyst |
| CN114669304B (en) * | 2021-12-31 | 2023-11-03 | 山东庚辰环保新材料有限公司 | Desulfurization catalyst and preparation method thereof |
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| CN101259366A (en) * | 2008-03-27 | 2008-09-10 | 史汉祥 | Oxidation method in flue gas desulfurization course |
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|---|
| 《滴流床反应器的研究现状和展望》;王蓉等;《化工进展》;19920531;10-16页 * |
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