CN1202903C - Process for desulfurizing fume - Google Patents
Process for desulfurizing fume Download PDFInfo
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- CN1202903C CN1202903C CN 01114170 CN01114170A CN1202903C CN 1202903 C CN1202903 C CN 1202903C CN 01114170 CN01114170 CN 01114170 CN 01114170 A CN01114170 A CN 01114170A CN 1202903 C CN1202903 C CN 1202903C
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- flue gas
- organic acid
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Abstract
The present invention relates to a method for smoke gas desulfuration, more specifically to a method synthetically utilizes industrial wastewater and waste slag to carry out wet type smoke gas desulfuration. In the method of the present invention, industrial wastewater and waste slag which contain organic acid and salt are added in a lime (stone) wet type smoke gas desulfuration system. Industrial wastewater which comprises little organic acid and salt but contains more other organic substances can be treated by wet type air oxidation. After the contents of organic acid or organic salt are increased, the industrial wastewater is added in a smoke gas desulfuration system. On one hand, the method of the present invention can enhance the smoke gas desulfuration rate and the utilization rate of lime (stone); on the other hand, the present invention synthetically utilizes valuable ingredients in industrial wastewater and waste slag, has no secondary pollution generated, and achieves the purpose of using waste to treat waste. The method of the present invention can be used for the smoke gas desulfuration process for various types of thionic oxides.
Description
The present invention relates to a kind of fume desulphurization method, particularly relate to a kind of waste water in oil plant, chemical plant etc. or method that waste residue carries out flue gas desulfurization of making full use of.
Oxysulfide is big, the wider a kind of gaseous contaminant of influence surface of quantity in the atmosphere pollution, the combustion process that mainly comes from coal and oil, and the roasting of sulfide ore, smelting process, wherein various boilers particularly power plant boiler smoke evacuation have characteristics such as sulfoxide concentration is low, exhaust gas volumn is big, floating dust is many and are difficult to improvement.Flue gas desulfurization technique can be divided into dry desulfurization and wet desulphurization in the prior art, because the desulfurization degree height of wet desulfurizing process, technology maturation and use in industry at most wherein are most widely used with wet type lime (stone) method.The advantage of lime (stone) method is that the raw sorbent cost is low, and subject matter is that the solubility of absorbent (lime or lime stone) is little, and utilization rate is low, and the waste residue amount is big, and when particularly adopting low-cost lime stone to be absorbent, this problem is more outstanding.
At the low problem of wet type lime (stone) method alkaline matter utilization rate, some solutions have been proposed in the prior art, mainly be in system, to add auxiliary agent with cushioning effect.Propose in the flue gas desulphurization system that with the lime stone is absorbent, to add the ammonium ion of 500～7500ppm as US5630991, improve the rate of dissolution of lime stone, therefore under the situation that reduces slurries internal circulating load and less calcium sulfur ratio, have higher desulfurization degree.Add organic acid and be used for flue gas wet type lime (stone) desulphurization system as buffer, write in the textbook as typical technology, introduced a kind of lime/lime stone wet desulphurization method of correction as " Air Pollution Control Engineering " the 334th～336 page of Higher Education Publishing House's publication in 1989, when adding 1～5kg adipic acid/t lime stone, under identical desulfurization degree, the utilization rate of lime stone can be brought up to more than 80% by 65～70%.It is that 4.5～6 solution carries out the flue gas wet type desulfurizing as absorption liquid with the pH value that contains organic acid such as formic acid, acetate, adipic acid or mixed organic acid that US5558848 discloses a kind of, regenerates with lime or lime stone in the pH value of the absorption liquid back that descends.US5693301 proposes a kind of lime or lime stone layer flue gas desulphurization system that adds weak organic acid that contain, and the pH value of wherein adding the desulfurization layer of weak organic acid is 3.0～5.5.Though such scheme can improve the utilization rate of absorbent, its subject matter is the cost height of additive, is unsuitable for large-scale flue gas desulphurization system.
In petroleum refining process, can discharge alkaline residue with sodium hydroxide solution detergent preparing petroleum products, according to the difference of the oil product of being made with extra care, alkaline residue can be further divided into normal top gasoline alkaline residue, a normal line alkaline residue, normal two wires alkaline residue, atmosphere 3rd side cut alkaline residue, catalytic gasoline alkaline residue, catalytic diesel oil alkaline residue, coker gasoline alkaline residue, coker gas oil alkaline residue, liquid hydrocarbon alkaline residue etc.These alkaline residues, mainly by free alkali, neutral oil, sodium naphthenate, phenol sodium, sulfide, compositions such as low molecular organic acids salt, wherein sodium naphthenate mainly is distributed in a normal line alkaline residue, normal two wires alkaline residue, in the atmosphere 3rd side cut alkaline residue, phenol sodium mainly is distributed in normal top gasoline alkaline residue and catalytic gasoline alkaline residue, the catalytic diesel oil alkaline residue, the coker gasoline alkaline residue, in the coker gas oil alkaline residue, sulfide then concentrates on normal top gasoline alkaline residue, the catalytic gasoline alkaline residue, the coker gasoline alkaline residue, the coker gas oil alkaline residue, in catalytic diesel oil alkaline residue and the liquid hydrocarbon alkaline residue, low molecular organic acids salt mainly is distributed in normal top gasoline alkaline residue, a normal line alkaline residue, in the normal two wires alkaline residue etc.From these alkaline residue compositions as can be known, if they are not dealt carefully with, will produce serious environmental and pollute.
Existing alkaline residue treatment technology mainly contains sulfuric acid neutralisation and carbon dioxide neutralisation.The alkaline residue N-process that reclaims aphthenic acids needs sulfuric acid acidation, and the water of generation is commonly referred to acid water because its pH value is lower, and contains more organic pollution, as low molecular organic acids etc., belong to harm big, handle the sewage of difficulty.Usually adopt to add in the alkali and discharging, or the method for discharging again after the solvent extraction processing.Contain more sodium carbonate in the carbodiimide solution that the carbon dioxide neutralisation produces, in the carbodiimide solution according to the difference of processing alkaline residue and contain the sulfide of different content usually, also contain more organic matter simultaneously, as low molecular organic acids, have certain solubility organic matter, do not separate emulsion etc. completely, its COD value can reach more than the 10000mg/l usually.The processing method of alkaline residue carbodiimide solution is mainly and adopts drying tower to reclaim wherein sodium carbonate, but because the cost recovery height, price is low and " unable to make ends meet " economically produces secondary pollution simultaneously owing to dried tail gas is seriously polluted.Also have with alkaline residue directly carry out wet oxidation remove wherein sulfide and part or all of COD to reach discharge standard or to handle preliminary treatment as biochemical treatment as other, but exhaustive oxidation technology has shortcomings such as condition harshness, equipment investment and operating cost height, though relax as pretreated wet-type oxidation technology condition, but need further to handle, long flow path, investment and operating cost are also not low, simultaneously, these two kinds of methods are not all utilized the valuable substance in the alkaline residue carbodiimide solution, can be described as a kind of waste of resource.
Also have the processing of some other waste water also to have the problems referred to above in the industrial production, as waste water of paper mill, Organic Chemicals factory effluent etc.
The object of the present invention is to provide that a kind of operating cost is low, the treatment of wastes with processes of wastes against one another, make full use of the fume desulphurization method of various valuable components in industrial wastewater or the waste residue.
The present invention is a kind of wet method lime or lime stone flue gas desulfurization technique, adds in desulphurization system and contains organic acid or acylate solution, and this organic acid or acylate solution come from industrial wastewater or waste residue.When industrial wastewater or waste residue organic acid or salt content less, and other organic matter more for a long time, in order to improve the content of acylate in industrial wastewater or the waste residue, industrial wastewater or waste residue can be carried out adding in the desulfurization absorbent again after the wet oxidation, oxidizing temperature is 150～260 ℃, be preferably 190～220 ℃, pressure is the pressure of liquid phase for keeping water, and oxidization time is 10 minutes～3 hours.Oxidant can be air, oxygen-enriched air or oxygen enrichment industrial waste gas etc., and wherein contained amount of oxygen is for alkaline residue or alkaline residue carbodiimide solution exhaustive oxidation being 0.2～5 times of carbon dioxide requisite oxygen amount.
Because principle of the present invention is the treatment of wastes with processes of wastes against one another, so the ratio that industrial wastewater or waste residue add in the absorbent can not done strict restriction.When exhaust gas volumn less and waste water or waste residue amount were big, the ratio of waste water or waste residue and lime or lime stone can be more greatly; When exhaust gas volumn big and waste water or waste residue amount more after a little while, can reduce the addition of waste water or waste residue.But in order to reach buffering effect preferably, organic acid content is preferably 0.5～4mmol/mol calcium in the absorption slurries, and when organic acid content reached above-mentioned scope in absorbing slurries, absorbent preferably adopted cheapest lime stone.
It is basic identical to add organic acid flue gas desulfurization condition in flue gas desulfurization technique condition and the prior art, but can suitably adjust operating condition in order to reach different purposes.As can suitably increasing calcium sulfur ratio in order to improve desulfurization degree, add big cycle volume, increasing gas residence time etc., but increasing calcium sulfur ratio can make the absorbent utilization rate low, add big cycle volume and can make equipment scale huge with the increase gas residence time, operating cost also correspondingly increases; As in order to improve the absorbent utilization rate, can reduce calcium sulfur ratio, but desulfurization degree is influenced.During practical application, can design as required.
Specify flue gas desulfurization scheme of the present invention below.
(1) flue gas desulfurization reactive moieties
Technology of the present invention can adopt common flue gas desulfurization flow process, and absorb slurries and in desulfurizing tower, contact certain hour with flue gas, the exhaust gas reheater discharging, slurries partly circulate, and part is discharged, and discharge section is through precipitation, and liquid phase is returned pulping system.Absorbent is selected lime stone or lime, owing to added organic acid or acylate, preferentially uses cheap lime stone, and the pH value of loop slurry is controlled at 3～7, is preferably 4～6.
(2) contain the source and the processing mode of organic acid or salting liquid
Principle of the present invention is the treatment of wastes with processes of wastes against one another, employed organic acid or the salting liquid of containing comes from waste water, the waste residue that oil refining, chemical industry and other production process produce, as in oil plant oil refinery alkaline residue, the oil refinery alkaline residue sulfuric acid and in the acid water, oil refinery alkaline residue carbon dioxide and carbodiimide solution, paper mill alkaline sewage etc.; Contain organic acid waste liquid such as Production of Terephthalic Acid waste water, acetic acid production process acid waste water etc. in the chemical process.If multiple source is arranged, also above-mentioned sewage can be mixed and use.Different waste water or waste residue because the pollutant kind difference that is wherein contained need be carried out suitable processing, and then add in the flue gas desulphurization system.For oil plant oil refinery alkaline residue, as catalytic gasoline alkaline residue, coker gas oil alkaline residue etc., can carry out wet oxidation earlier, to reach the purpose that increases organic acid content and deodorization, contact in advance with flue gas then, isolate organic facies, aqueous phase contains more materials such as small molecular organic acid, adds flue gas desulfurization and absorbs in the slurries.For in the sulfuric acid of oil plant oil refinery alkaline residue and acid water, because its pH value is lower, the organic matter separation is comparatively complete, and not isolated organic matter mostly is small molecular organic acid, can directly add in the flue gas desulfurization absorbent.For in the carbon dioxide of oil plant oil refinery alkaline residue and carbodiimide solution, because the pH value is higher, can contact in advance with flue gas earlier, add again in the flue gas desulfurization absorbent after isolating organic facies; Also carbodiimide solution can be carried out wet oxidation, increase small molecular organic acid content, reduce other organic content, and then add in the desulfurization absorbent.For the paper mill alkaline sewage, owing to wherein contain organic acid seldom, before adding the desulfurization vapor, must carry out wet oxidation earlier, make wherein to produce small molecular organic acid.For containing organic acid waste water, as Production of Terephthalic Acid waste water, acetic acid production waste water etc., because wherein organic matter majority exists with the small molecular organic acid form, so can directly add in the flue gas desulphurization system.The purpose of above-mentioned wet oxidation process is to increase wherein organic acid or acylate content.For reducing corrosion, oxidizing process is preferably under the alkali condition carries out, oxidizing condition is controlled under the condition of production of organic acids maximum the most favourable, under at 200～210 ℃, 3～4MPa pressure, with air oxidation paper mill black liquor, wherein organic 70%～90% can be oxidized to low molecular organic acids.The tail gas of oxidizing process can with smoke evacuation tail gas dual disposal.
(3) contain the adding mode of organic acid or salting liquid
For oil refinery alkaline residue after oil refinery alkaline residue carbodiimide solution or the wet oxidation etc., can be used for the flue gas pre-wash earlier, the solution after the pre-wash adds in the absorbent slurry again.Made full use of basicity wherein (sodium carbonate) like this, can further remove most of organic matter in the alkaline residue on the other hand, prevented that these organic matters from sticking to the pulpous state absorbent surface, influences the utilization rate of absorbent.Simultaneously, for oil refinery alkaline residue carbodiimide solution, when it mixes with the calcium hydroxide absorbent, can also prevent to produce precipitation of calcium carbonate.For in the oil refinery alkaline residue sulfuric acid and acid water, contain paper mill alkaline sewage after organic acid wastewater or the wet oxidation etc., can directly add in the absorption liquid or be used for absorbent slurrying.Contain organic acid or salting liquid and can add reaction system continuously, also can add in the desulphurization reaction system by batch (-type).
(4) organic acid content is kept situation in the desulphurization system
Low molecular organic acids or its salt are lyotrope matter, effluxing organic acid contained in the slurries or salt major part is present in the waste residue dehydration clear liquid, because this clear liquid reuse can make most of organic acid be recycled, the organic acid that loses from efflux slurries is less.Another loss of organic acid is oxidation, because the oxidation air that generally contains the remaining oxygen in the combustion process or feed in the flue gas in order to produce gypsum, oxidation reaction will take place and lose in organic acid in containing the oxygen system, it is lower to reach temperature owing to oxygen content in the desulphurization system is low, and oxidation is not fairly obvious.Evaporation also will be lost the part organic acid in addition.Therefore, for keeping finite concentration, need be in system continuously or batch (-type) replenish waste residue or the waste water that contains organic acid or salt on a small quantity.
The present invention is that additive carries out lime (stone) wet process of FGD according to the principle of the treatment of wastes with processes of wastes against one another with industrial wastewater, waste residue, has improved flue gas desulphuization rate on the one hand, has improved the absorbent utilization rate, has reduced operating cost, reduces waste residue output; Solved the handling problem of waste water on the other hand, made that various valuable components have all obtained utilization in the waste water.Can be widely used in various types of flue gas desulfurization courses, be specially adapted to produce in the flue gas desulfurization course of boiler in above-mentioned waste water, the waste residue factory.
Further specify the solution of the present invention and effect below in conjunction with embodiment, wherein the COD value is the chromium method.
Embodiment 1
The oil plant catalytic gasoline is made with extra care alkaline residue carbodiimide solution, COD 32000mg/L; Phenol 12200mg/L; The pH value is 8.8.Wet type liquid phase oxidation condition: 190 ℃ of oxidizing reaction temperatures, reaction pressure 2.8MPa, spent lye are at the void tower time of staying of oxidation reactor 1.2h, and air capacity is 3 times of exhaustive oxidation requirement.After the oxidation in the alkaline residue organic acid content be 0.5mol/l, be mainly low molecular organic acids such as formic acid, acetate, propionic acid, butyric acid, 3 Methylbutanoic acid, 2 methyl valeric acid, caproic acid etc.Carbodiimide solution after the oxidation is used for the lime stone slurrying of lime stone wet flue gas desulfurization, and agstone is 200 orders.Organic acid content is a 3mmol/mol calcium in the loop slurry, and solids content is 10%, and the pH value is 5.4, and total calcium sulfur ratio (mole) is 1.1, and liquid-gas ratio is 7l/m
3Flue gas, gas-liquid contact (hollow-spraying-tower) time is 7 seconds.Import SO 2 from fume concentration is 3700 μ l/l, and desulfurization degree is 93%, and the lime stone utilization rate is 85%.
Embodiment 2
Oil plant is normal one, in the refining alkaline residue sulfuric acid in two wires and acid water, COD 9483mg/L; Phenol 102mg/L; The pH value is 2.6.Acid water is used for the slurrying of lime stone wet flue gas desulfurization, and agstone is 325 orders.Organic acid content is a 0.5mmol/mol calcium in the loop slurry, and solids content is 12%, and the pH value is 5.4, and total calcium sulfur ratio is 1.2, and liquid-gas ratio is 6l/m
3Flue gas, gas-liquid contact (hollow-spraying-tower) time is 7 seconds.The import flue gas concentration is 2400 μ l/l, and desulfurization degree is 95%, and the lime stone utilization rate is 80%.
Embodiment 3
Oil plant oil refinery mixing alkaline residue, COD 492880mg/L; Phenol 1663mg/L; The pH value is 14.This alkaline residue contacts with flue gas and carries out the pre-desulfurization of flue gas, and the pH value reaches alkaline residue discharge in 4 o'clock and carries out static layering, and organic layer goes to reclaim and purifies, and water layer is directly used in lime slurrying.Organic acid content is a 0.5mmol/mol calcium in the loop slurry, and solids content is 12%, and the pH value is 5.6, and total calcium sulfur ratio is 1.0, and liquid-gas ratio is 7l/m
3Flue gas, gas-liquid contact (hollow-spraying-tower) time is 7 seconds.The import flue gas concentration is 1500 μ l/l, and desulfurization degree is 94%, and the lime utilization rate is 94%.
Embodiment 4
Alkaline residue among the embodiment 3 carries out wet oxidation, 240 ℃ of oxidizing reaction temperatures, and reaction pressure 4.5MPa, spent lye are at the void tower time of staying of oxidation reactor 0.4h, and air capacity is 0.8 times of exhaustive oxidation requirement.The pH value of alkaline residue is 13.2 after the oxidation, and acylate content is 8.2mol/l.This alkaline residue contacts with flue gas and carries out the pre-desulfurization of flue gas, and the pH value reaches alkaline residue discharge in 4 o'clock and carries out static layering, and organic layer goes to purify, and water layer is directly used in lime stone slurrying, and agstone is 325.Organic acid content is a 5mmol/mol calcium in the loop slurry, and solids content is 12%, and the pH value is 5.6, and total calcium sulfur ratio is 1.0, and liquid-gas ratio is 6l/m
3Flue gas, gas-liquid contact (hollow-spraying-tower) time is 7 seconds.The import flue gas concentration is 3700 μ l/l, and desulfurization degree is 93%, and the lime stone utilization rate is 93%.
Embodiment 5
Alkaline residue carbodiimide solution among the embodiment 1 contacts in advance with flue gas, when the pH value reaches 4, isolates organic facies, and water adds in the lime flue gas desulphurization system, adds from loop slurry.Organic acid content is a 1mmol/mol calcium in the loop slurry, and solids content is 12%, and the pH value is 6.4, and total calcium sulfur ratio is 1.0, and liquid-gas ratio is 8l/m
3Flue gas, gas-liquid contact (hollow-spraying-tower) time is 7 seconds.The import flue gas concentration is 1800 μ l/l, and desulfurization degree is 95%, and the lime utilization rate is 95%.
Embodiment 6
The paper mill black liquor, COD 47200mg/l, pH value 11.4 is added sodium carbonate, makes to contain sodium carbonate 23% in the black liquor, then at 210 ℃, carries out air oxidation 2 hours under the 4MPa, and air capacity is 1.2 times of exhaustive oxidation requirement.Contain organic hydrochlorate 1.4mol/l after the oxidation in the solution.This solution is used for lime stone slurrying, and agstone is 325 orders.Organic acid content is a 2mmol/mol calcium in the loop slurry, and solids content is 12%, pH value 5.6, total calcium sulfur ratio 1.1, liquid-gas ratio 6l/m
3Flue gas, gas-liquid 7 seconds (hollow-spraying-tower) time of contact.Import flue gas concentration 3000 μ l/l, desulfurization degree 94%, lime stone utilization rate 85%.
Embodiment 7
P-phthalic acid's factory effluent, COD is 9800mg/L, is mainly acetate and terephthalic acid (TPA), and this waste water adds in the loop slurry of lime stone wet flue gas desulfurization, and agstone is 325 orders.Organic acid content is a 2mmol/mol calcium in the loop slurry, and solids content is 12%, and the pH value is 5.5, and calcium sulfur ratio is 1.1, and liquid-gas ratio is 7l/m
3Flue gas, gas-liquid contact (hollow-spraying-tower) time is 7 seconds.The import flue gas concentration is 1000 μ l/l, and desulfurization degree is 96%, and the lime stone utilization rate is 87%.
Comparative example
The flue gas desulfurization operating condition is identical with embodiment 1, just absorbs alkali-free slag oxidation waste liquid in the slurries, and desulfurization degree is 75% as a result, and the lime stone utilization rate is 68%.
Claims (9)
1, a kind of lime or lime stone wet method fume gas desulfurizing method, in desulphurization system, add and contain organic acid or acylate solution, it is characterized in that this organic acid or acylate solution come from industrial wastewater or waste residue, described industrial wastewater or waste residue are in the sulfuric acid of oil refinery alkaline residue, oil refinery alkaline residue and the carbon dioxide of acid water, oil refinery alkaline residue in and carbodiimide solution, paper mill alkaline sewage and contain a kind of or composite waste in the organic acid wastewater.
2, in accordance with the method for claim 1, it is characterized in that described oil refinery alkaline residue earlier through wet oxidation, contacts with flue gas more in advance, add in the flue gas desulphurization system after isolating organic facies.
3, in accordance with the method for claim 1, it is characterized in that in the sulfuric acid of described oil refinery alkaline residue and acid water directly adds in the flue gas desulphurization system.
4, in accordance with the method for claim 1, it is characterized in that contacting in advance with flue gas earlier with carbodiimide solution in the carbon dioxide of described oil refinery alkaline residue, isolate after the organic facies in the adding flue gas desulphurization system.
5, in accordance with the method for claim 1, it is characterized in that in the carbon dioxide of described oil refinery alkaline residue and after carbodiimide solution carries out wet oxidation earlier, add in the flue gas desulphurization system again.
6, in accordance with the method for claim 1, it is characterized in that described paper mill alkaline sewage adds in the flue gas desulphurization system through after the wet oxidation earlier again, oxidizing temperature is 200～210 ℃, and pressure is 3～4MPa.
7, in accordance with the method for claim 1, it is characterized in that the described organic acid wastewater that contains directly adds in the flue gas desulphurization system.
8, according to claim 2,5 or 6 described methods, it is characterized in that described wet oxidation condition is: oxidizing temperature is 150～260 ℃, pressure is the pressure of liquid phase for keeping water, oxidization time is 10 minutes～3 hours, oxidant is air, oxygen-enriched air or oxygen enrichment industrial waste gas, and contained amount of oxygen is for industrial wastewater or waste residue exhaustive oxidation being 0.2～5 times of carbon dioxide requisite oxygen amount.
9, in accordance with the method for claim 1, it is characterized in that described organic acid or salt are 0.5～4mmol/mol calcium at the content that desulfurization absorbs in the slurries.
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| CN 01114170 CN1202903C (en) | 2001-07-02 | 2001-07-02 | Process for desulfurizing fume |
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| CN101417729B (en) * | 2007-10-26 | 2010-12-22 | 中国石油化工股份有限公司 | Method for protecting storage tank by using flue gas |
| AU2009352300B2 (en) * | 2009-09-14 | 2014-01-23 | Joseph Daniel Cook | Method for wet flue gas desulfurization |
| CN102000491A (en) * | 2010-11-18 | 2011-04-06 | 华北电力大学（保定） | Combined synergist for wet flue gas desulfurization process and use method thereof |
| CN102091510B (en) * | 2010-12-17 | 2013-09-04 | 马鞍山市鸿伟环化有限公司 | Flue gas desulfurization synergist and using method thereof |
| CN102489133A (en) * | 2011-12-06 | 2012-06-13 | 江西省电力科学研究院 | Desulfurization slurry stabilizing agent for wet limestone flue gas desulfurization, and using method of desulfurization slurry stabilizing agent |
| CN102941008B (en) * | 2012-11-21 | 2015-04-29 | 北京化工大学 | Method for absorbing SO2 by soluble calcium saline solution and regenerating absorbent |
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