CN102872718A - Oxidation method of wet flue gas desulfurizing liquid - Google Patents
Oxidation method of wet flue gas desulfurizing liquid Download PDFInfo
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- CN102872718A CN102872718A CN2011101927834A CN201110192783A CN102872718A CN 102872718 A CN102872718 A CN 102872718A CN 2011101927834 A CN2011101927834 A CN 2011101927834A CN 201110192783 A CN201110192783 A CN 201110192783A CN 102872718 A CN102872718 A CN 102872718A
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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, especially relate to catalytic oxidation technology and the employed catalyst thereof of sulphite in the wet process of FGD liquid.
Background technology
During combustion of sulfur fuel, except a part of sulphur is contained in the cigarette ash, other parts will be thrown into atmosphere with the form of sulfur dioxide.Sulfur dioxide not only works the mischief to health, but also can form acid rain, and environment is caused serious pollution.Therefore, large-scale burner is generally all equipped flue gas desulfur device, and wherein majority is wet flue gas desulfurizer.
Usually mainly containing sulphite in the doctor solution that obtains after the wet desulphurization, for the ease of the utilization of sulphite and make the wastewater to reach standard of discharging, need to be sulfate with sulfite oxidation.Industrial common employing arranges storage tank at the bottom of the absorption tower, the doctor solution that stores in the storage tank passes into air, oxidation sulphite with the form of bubbling.But this mode oxidation rate is very slow, and transforming 90% such as calcium sulfite probably needs 4～5 hours; Magnesium sulfite transforms 90% needs 7～8 hours.Therefore, desulfurization product usually precipitates owing to oxidation rate reaches capacity in absorption liquid slowly very soon.In addition, the COD of efflux wastewater also usually is higher than national standard.
CN101259366A discloses a kind of method for oxidation in the flue gas desulfurization course.Promote that by three kinds of modes sulfite oxidation is sulfate in the doctor solution: the one, directly in flue gas, pass into air; The 2nd, in absorption equipment, establish in addition an air delivery pipe, air is sent into flue gas and is mixed in the absorption tower; The 3rd, at gas and liquid flowing and under situation under, pass into air in " slurries " agent exit, by the Liqiud-gas mixing device that arranges, air and " slurries " are mixed.
CN1565709A discloses a kind of catalytic oxidation technique of flue gas desulfurization product, at flue gas SO
2Add an amount of soluble salts catalyst in the absorption liquid, when containing 0.001 ~ 0.02mol/L catalyst in the absorption liquid, desulfurization product reaches more than 90.6% at 2 hours conversion ratio.CN101244360A discloses a kind of catalytic oxidation technique of calcium sulfite, and this technique is absorbing SO
2After slurries in add soluble ferric iron salt, manganese salt or the two mixture as catalyst.More than 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 replenish 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 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 behind a kind of smoke-gas wet desulfurization, this technique is simple, and operating cost is low, non-secondary pollution, catalyst has good catalytic activity and stability to the oxidation of the sulphite in the doctor solution.
A kind of catalysed oxidation processes of flue gas desulfurization liquid is characterized in that making absorption SO
2After doctor solution and air enter continuously the fixed bed reactors that catalyst is housed, in the presence of oxidation catalyst, carry out oxidation reaction.
According to catalysed oxidation processes of the present invention, described doctor solution and oxygen can pass through fixed bed reactors in the mode that also flows.Doctor solution as described and air enter reactor from the top of reactor, catalyst exist and suitable oxidizing condition under, by fixed bed reactors, the reaction afterproduct leaves reactor from reactor bottom with downflow system; Perhaps doctor solution and air enter reactor from reactor bottom, catalyst exist and suitable oxidizing condition under, by fixed bed reactors, reacted product leaves reactor from reactor top in the upper reaches mode.
According to catalysed oxidation processes of the present invention, described course of reaction can be the counter-current operation mode: doctor solution enters reactor from reactor head, oxygen enters reactor from reactor bottom, under the existence of catalyst and suitable oxidizing condition, passes through fixed bed reactors in the mode of adverse current.
The operating condition of doctor solution oxidation reaction is: doctor solution volume air speed is 0.1 ~ 10h
-1, preferred 0.5 ~ 5h
-1Air/doctor solution volume ratio is 5～200, preferred 10 ~ 100; In the inventive method, reaction temperature and pressure need not controlled, and the doctor solution temperature and pressure that discharges during by the flue gas desulfurization normal operating gets final product.
Wherein said absorption SO
2The composition of doctor solution according to the difference of absorbent in the flue gas desulfurization course and difference.Generally comprise one or more in sodium sulfite, magnesium sulfite and the calcium sulfite in the doctor solution.The concentration of sulphite is 0.1g/L ~ 100g/L in the doctor solution, and doctor solution pH value is 4 ~ 8.
Wherein said oxidation catalyst is the 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 the samarium oxide.Take the weight of catalyst as benchmark, the 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: at first ceramic honey comb matrix dipping is contained aluminium oxide, zirconia, titanium oxide or the slurries of two or three composite oxides wherein, take out, blow away unnecessary slurries in the duct, drying and roasting make the ceramic honey comb of coated carrier coating; Next will apply the salting liquid of the ceramic honey comb dipping rare earth metal of good vector coating, and take out, and blow away unnecessary slurries in the duct, drying and roasting can prepare this catalyst.
Compared with prior art, the method for oxidation of smoke-gas wet desulfurization liquid of the present invention has following advantage:
1, this method has improved the oxidation rate of sulphite, effectively reduces sulphite in intrasystem deposition.When especially adopting the desulfurization of magnesium method, because the solubility of magnesium sulfite is very little, the oxidation rate of magnesium sulfite is slow in the existing technique, 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 has been avoided the appearance of sediment much larger than magnesium sulfite.
2, this method has improved the oxygenation efficiency of sulphite, and makes the COD of desulfurization efflux wastewater up to standard.For adopting the desulfurization of 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, it is typically used as catalyst carrier, such as Fe
2O
3/ CeO
2Catalyst.And in the inventive method, the applicant is unexpected to be found, adopts rare-earth oxide as the catalyst activity metal component, and the gained catalyst has good catalytic oxidation performance equally, can satisfy the needs of sulfite oxidation in the doctor solution fully.Particularly valuable is that rare-earth metal catalyst is the loss of inactive component in use, can reuse, thereby reduce running cost, also can effectively avoid the secondary pollution of running off and causing because of active metal component.And in the prior art, as adopting soluble manganese salt as catalyst oxidation sweetening liquid among the patent CN1565709A, the concentration of described soluble manganese salt in doctor solution is more than 0.001mol/L.After the doctor solution oxidation, the manganese that contains in the doctor solution is up to more than the 275mg/L, much larger than the country " sewage drainage standard " in the regulation total manganese discharge standard (＜5mg/L), brought new secondary pollution, need subsequent process to reclaim or remove manganese in the doctor solution, complex treatment process, operating cost is high.
The advantages such as 4, solid catalyst of the present invention is that ceramic honeycomb catalyst has the mechanical strength height, and wear-resistant, fluid resistance is little, and the life-span is long.
The specific embodiment
The specific embodiment of the present invention will be carried out exemplary explanation in more detail by following examples, and described embodiment should not be construed as the restriction of the scope of the invention.
ZrO among the embodiment
2, TiO
2Be the commercially available prod with boehmite, used cerous nitrate, lanthanum nitrate, samaric nitrate etc. are chemically pure reagent.
Embodiment 1
The preparation of doctor solution oxidation catalyst:
(1) preparation of coating slurries
With 20 gram ZrO
2, 20 the gram TiO
2Mix rear adding 240 ml deionized water and stirring with 8 gram boehmites, place the ball mill ball milling namely to get required coating slurries above-mentioned mixed serum.
(2) the coating slurries apply
63.15 gram cordierite honeycomb ceramic matrixes are immersed in the coating slurries that step (1) configures, blow away the raffinate in the duct after the taking-up, 100 ℃ of dryings 5 hours, 500 ℃ of roastings 5 hours.
(3) load of active component
Taking by weighing 18 gram cerous nitrates and 28 gram lanthanum nitrates are dissolved in the 500ml deionized water, will apply in the step (2) in the sample dipping mentioned solution of coating, take out, blow away raffinate, 100 ℃ of dryings 2 hours 500 ℃ of roastings 5 hours, can make 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%, and active component CeLa content is 5wt%, and Ce/La is 1:2.
The doctor solution oxidation:
Concentration of sodium sulfite is 2200 mg/L in the doctor solution, and COD is 432 mg/L, and the 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 from reactor bottom, at CeLa/TiO
2-ZrO
2-Al
2O
3React under the catalytic action of/CH catalyst (catalyst volume 100mL).Reaction condition is: doctor solution volume air speed is 3 h
-1, reaction temperature is 45 ℃, air/doctor solution volume ratio is 200.After question response is stablized 60 minutes, sample analysis ion concentration of inferior sulfate radical and COD.
Embodiment 2
Preparation method according to embodiment 1 prepares Ce/ZrO
2/ CH, wherein coated carrier ZrO
2Proportion is 5 wt%, and active component Ce content is 1 wt% catalyst.
The doctor solution oxidation:
Concentration of sodium sulfite is 2670 mg/L in the doctor solution, and COD is 512 mg/L, and the 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 from reactor bottom, at Ce/ZrO
2React under the catalytic action of/CH catalyst (catalyst volume 100mL).Reaction condition is: doctor solution volume air speed is 4 h
-1, reaction temperature is 54 ℃, air/doctor solution volume ratio is 100.After question response is stablized 60 minutes, sample analysis ion concentration of inferior sulfate radical and COD.
Embodiment 3
Preparation method according to embodiment 1 prepares Pr/ZrO
2/ CH, wherein coated carrier ZrO
2Proportion is 10 wt%, and active component Pr content is 3 wt% catalyst.
The doctor solution oxidation:
Concentration of sodium sulfite is 2860 mg/L in the doctor solution, and COD is 548 mg/L, and the 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 from reactor bottom, at Pr/ZrO
2React under the catalytic action of/CH catalyst (catalyst volume 100mL).Reaction condition is: doctor solution volume air speed is 1h
-1, reaction temperature is 55 ℃, air/doctor solution volume ratio is 10.After question response is stablized 60 minutes, sample analysis ion concentration of inferior sulfate radical and COD.
Embodiment 4
Adopt the CeLa/TiO of embodiment 1 preparation
2-ZrO
2-Al
2O
3/ CH catalyst.
The doctor solution oxidation:
Concentration of sodium sulfite is 4311 mg/L in the doctor solution, and COD is 710 mg/L, and the 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 pass through fixed bed reactors under flowing to.Reaction condition is: doctor solution volume air speed is 0.5h
-1, reaction temperature is 50 ℃, air/doctor solution volume ratio is 80.After question response is stablized 60 minutes, sample analysis ion concentration of inferior sulfate radical and COD.
Embodiment 5
Adopt the CeLa/TiO of embodiment 1 preparation
2-ZrO
2-Al
2O
3/ CH catalyst.
The doctor solution oxidation:
Doctor solution Central Asia magnesium sulfate concentration is 3132 mg/L, and COD is 588 mg/L, and the 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 air speed is 1.8h
-1, reaction temperature is 48 ℃, air/doctor solution volume ratio is 20.After question response is stablized 60 minutes, sample analysis ion concentration of inferior sulfate radical and COD.
Embodiment 6
The preparation of catalyst: the preparation method according to embodiment 1 prepares Sm/TiO
2-ZrO
2/ CH, wherein coated carrier TiO
2-ZrO
2Proportion is 15wt%, and active component Sm content is 8wt%.
The doctor solution oxidation:
Doctor solution Central Asia calcium sulfate concentration is 145 mg/L, and COD is 95 mg/L, and the 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 air speed is 1.8h
-1, reaction temperature is 40 ℃, air/doctor solution volume ratio is 200.
Embodiment 7
Preparation method according to embodiment 1 prepares Nd/TiO
2/ CH catalyst, wherein coated carrier TiO
2Proportion is 30 wt%, and active component Nd content is 10 wt%.
The doctor solution oxidation:
Concentration of sodium sulfite is 92000 mg/L in the doctor solution, and COD is 18900 mg/L, and the 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 air speed is 0.1h
-1, reaction temperature is 65 ℃, air/doctor solution volume ratio is 150.After question response is stablized 60 minutes, sample analysis ion concentration of inferior sulfate radical and COD.
Embodiment 8
Preparation method according to embodiment 1 prepares Ce/ZrO
2-Al
2O
3/ CH catalyst, wherein coated carrier ZrO
2-Al
2O
3Proportion is 20 wt%, and active component Ce content is 5 wt%.
The doctor solution oxidation:
Concentration of sodium sulfite is 80000 mg/L in the doctor solution, and COD is 16500 mg/L, and the 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 air speed is 2 h
-1, reaction temperature is 50 ℃, air/doctor solution volume ratio is 80.After question response is stablized 60 minutes, sample analysis ion concentration of inferior sulfate radical and COD.
Embodiment 9
Preparation method according to embodiment 1 prepares CeSm/Al
2O
3/ CH catalyst, wherein coated carrier Al
2O
3Proportion is 12 wt%, and active component CeSm content is 1 wt%, and Ce/Sm is 2:1.
The doctor solution oxidation:
Concentration of sodium sulfite is 1200 mg/L in the doctor solution, and COD is 320 mg/L, and the 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 air speed is 5 h
-1, reaction temperature is 55 ℃, air/doctor solution volume ratio is 50.After question response is stablized 60 minutes, sample analysis ion concentration of inferior sulfate radical and COD.
Comparative Examples 1
Except not adding catalyst, the other the same as in Example 1.
Comparative Examples 2
Doctor solution forms identical with embodiment 3.In doctor solution, add MnSO
4, as the Mn that adds
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 contain the Mn that concentration is 275mg/L in the doctor solution after the oxidation, much larger than the country " sewage drainage standard " in the regulation total manganese discharge standard (＜5mg/L), bring new secondary pollution, need subsequent process to reclaim or remove manganese in the doctor solution, make its treatment process more complicated, the operating cost height.
Reaction result sees Table 1.
The oxidation results of table 1 sulphite
| Embodiment and Comparative Examples | The sulfite oxidation rate, % | COD，mg/L |
| Embodiment 1 | 98.5 | 74 |
| Comparative Examples 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 (9)
1. a flue gas desulfurization liquid catalysed oxidation processes is characterized in that making absorption SO
2After doctor solution and air enter continuously the fixed bed reactors that catalyst is housed, in the presence of oxidation catalyst, carry out oxidation reaction, the operating condition of doctor solution oxidation reaction is: doctor solution volume air speed is 0.1 ~ 10h
-1, air/doctor solution volume ratio is 5～200.
2. according to catalysed oxidation processes claimed in claim 1, it is characterized in that described doctor solution and oxygen pass through fixed bed reactors in the mode that also flows.
3. according to catalysed oxidation processes claimed in claim 2, it is characterized in that described doctor solution and air enter reactor from the top of reactor, catalyst exist and suitable oxidizing condition under, by fixed bed reactors, the reaction afterproduct leaves reactor from reactor bottom with downflow system.
4. according to catalysed oxidation processes claimed in claim 2, it is characterized in that, described doctor solution and air enter reactor from reactor bottom, catalyst exist and suitable oxidizing condition under, by fixed bed reactors, reacted product leaves reactor from reactor top in the upper reaches mode.
5. according to catalysed oxidation processes claimed in claim 1, it is characterized in that described doctor solution enters reactor from reactor head, oxygen enters reactor from reactor bottom, under the existence of catalyst and suitable oxidizing condition, pass through fixed bed reactors in the mode of adverse current.
6. according to catalysed oxidation processes claimed in claim 1, it is characterized in that the operating condition of doctor solution oxidation reaction is: doctor solution volume air speed is 0.5 ~ 5h
-1Air/doctor solution volume ratio is 10 ~ 100.
7. according to catalysed oxidation processes claimed in claim 1, it is characterized in that described doctor solution comprises one or more in sodium sulfite, magnesium sulfite and the calcium sulfite, the concentration of sulphite is 0.1g/L ~ 100g/L in the doctor solution, and doctor solution pH value is 4 ~ 8.
8. according to catalysed oxidation processes claimed in claim 1, it is characterized in that, described oxidation catalyst is the 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 the samarium oxide.
9. according to catalysed oxidation processes claimed in claim 8, it is characterized in that take the weight of catalyst as benchmark, the coated carrier proportion is 5 ~ 30%, the content of active metal component counts 1% ~ 10% with metal.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106745155A (en) * | 2016-11-29 | 2017-05-31 | 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 |
| CN111389467A (en) * | 2020-03-19 | 2020-07-10 | 河北中垒新能源科技有限公司 | Limestone-gypsum wet desulphurization catalyst |
| CN114669304A (en) * | 2021-12-31 | 2022-06-28 | 山东庚辰环保新材料有限公司 | Desulfurization catalyst and preparation method thereof |
Citations (1)
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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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2011
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101259366A (en) * | 2008-03-27 | 2008-09-10 | 史汉祥 | Oxidation method in flue gas desulfurization course |
Non-Patent Citations (1)
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| 王蓉等: "《滴流床反应器的研究现状和展望》", 《化工进展》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106745155A (en) * | 2016-11-29 | 2017-05-31 | 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 |
| CN111389467A (en) * | 2020-03-19 | 2020-07-10 | 河北中垒新能源科技有限公司 | Limestone-gypsum wet desulphurization catalyst |
| 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 |
| CN114669304A (en) * | 2021-12-31 | 2022-06-28 | 山东庚辰环保新材料有限公司 | Desulfurization catalyst and preparation method thereof |
| 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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