CN101607173B - Desulfurization process of flue gas or waste gas by using external regenerative cycle magnesium sulfate method - Google Patents
Desulfurization process of flue gas or waste gas by using external regenerative cycle magnesium sulfate method Download PDFInfo
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Abstract
The invention relates to a desulfurization process of flue gas or waste gas by using an external regenerative cycle magnesium sulfate method. The flue gas or the waste gas containing sulfur dioxide is continuously introduced into an absorbing tower, the sulfur dioxide in the flue gas or the waste gas is absorbed by circularly spraying magnesium sulfite absorbing liquid, the magnesium sulfite in the absorbing liquid is transformed into magnesium bisulfite, the sulfur dioxide in the flue gas or the waste gas is removed, the absorbing liquid at the bottom of the absorbing tower is partially or fully shunted to enter in a regeneration system outside the tower and reacts with magnesium oxide slurry for regeneration, the obtained regenerative liquid is filtered, the magnesium sulfite solid is recovered, the filtrate is returned backed to the absorbing tower for cycle absorption and the sulfur dioxide in the flue gas or the waste gas is continuously removed. Due to the adoption of the regeneration process of the absorbing liquid, the pH value of the regeneration reaction end point and the transformation ratio of the agent are increased, the temperature of the absorbing liquid is reduced, the absorbing liquid has the characteristics of high pH value (7.2-8.5), low temperature (38-48 DEG C) and high absorbing capacity and the absorbent activity of the absorbing liquid is effectively improved.
Description
Technical field
The present invention relates to flue gas desulfurization technique, especially relate to the magnesium sulfite wet fuel gas desulfurizing technology.
Background technology
Flue gas desulfurization by magnesia wet method technology is succeeded in developing by U.S. Kai Mike basis company the earliest the sixties in last century; Philadelphia Electric after the seventies (PECO) and United & Constructor joint study magnesia method of reproduction sulfur removal technology; Through after several thousand hours the trial run; (wherein two are respectively 150MW and 320MW) dropped into FGD system and two magnesia regenerative systems of full scale on three generating sets; Said system was built up and is put into operation in nineteen eighty-two, and later stoppage in transit sulfuric acid manufactory in 1992 directly sells product magnesium sulfate.Binzhou, domestic Shandong 2 * 240t/hr boiler flue gas desulfurization has adopted the magnesium oxide method sulfur removal technology.
The principle of flue gas desulfurization by magnesia wet method is magnesia to be carried out digestion reaction generate magnesium hydroxide; Process certain density magnesium hydroxide and absorb slurries; The reaction of magnesium hydroxide and sulfur in smoke generates magnesium sulfite and magnesium bisulfite in the absorption tower; The part magnesium bisulfite that generates continues to generate magnesium sulfite with the magnesium hydroxide reaction in the absorption tower, and the mix slurry that reaction generates is proceeded circulation and absorbed.Final disposal approach by its desulfurization product magnesium sulfite is divided into magnesium sulfate method and magnesia method of reproduction; Its difference is that the former carries out oxidation with the magnesium sulfite bubbling air in tower that generates, and after the circulating absorption solution magnesium sulfate concentration reaches 7-8%, discharges in the tower and carries out subsequent treatment; The magnesium sulfite solid slurry that contains that the latter will generate is discharged in the absorption tower, control circulation fluid solid content 7-10%, and the magnesium sulfite solid of discharge carries out high-temperature roasting after drying and other treatment, reclaim magnesia and sulfur dioxide.Owing to of the restriction of conditions such as the regenerative response mixability that receives regenerative response system in the tower, the time of staying to the regenerative response degree; For guaranteeing the conversion ratio of magnesium hydroxide; Its regenerative response carries out under the excessive condition of magnesium bisulfite, and the condition of its regenerative response PH control is PH:5.8-6.5.In above-mentioned PH interval; Structure and sulfur dioxide inlet concentration according to the absorption tower; The liquid-gas ratio of control absorption process is 3-5 liter (absorption liquid)/mark cubic meter (gas), 50 ℃-55 ℃ of absorption liquid temperature, desulphurization system flue gas crushing 1200-2000Pa; Magnesium sulphur is than 1.1-1.2: 1, and desulfuration efficiency is greater than 90%.
The patent of at present domestic and international magnesium oxide method and the significant improvement that document does not relate to reaction mechanism and technology; Domestic patent " a kind of magnesia flue gas desulfurization and the oxidation of product thick slurry process reclaim technology " (CN1762550A) (CN1481926A) has proposed to adopt flue gas recirculation to carry dense reclaim sulfuric acid magnesium respectively from the angle of reclaim sulfuric acid magnesium with " a kind of flue gas desulfurization by magnesia wet method and product reclaim new technology " and has proposed the technology that the underflow oxidation generates magnesium sulfate with adopting in the absorption tower, do not relate to the improvement to flue gas desulfurization absorption and regeneration of absorption solution technology." the continuous reclaiming method of a kind of exhuast gas desulfurization, defluorinating absorbent liquid " of inventor's invention though (CN200610098180.7) sulfur method is improved to some extent, also needs NaOH, sodium carbonate, sodium acid carbonate or sodium sulfite.
China's magnesite reserves the first in the world, purity height, desulfurization material light-burning magnesium powder are the product after the simple calcining of magnesite, relative low price, and the magnesium oxide method desulfurization has huge resources advantage in China for this reason; In flue gas desulfurization course; Because the solubility of the neutralization reaction speed of magnesia and acid solution and formation sulphite is all greater than the calcium method; In the comprehensive utilization of absorption reaction speed, absorptivity, liquid-gas ratio, power consumption, waste residue and tower, all show bigger advantage aspect the preventing of fouling, this method has become the optimised process of present replace lime-gypsum method.But this method is owing to prolong the method for having used regeneration in the lime-gypsum method circulating absorption solution tower; Though aspect project occupation of land, process equipment and lime stone-gypsum method compatible, possess certain advantage; But because regenerative response receives solid-liquid to mix the restriction of conditions such as degree, reaction time in the tower; For keeping its higher regenerative response and oxidizing reaction rate and raising raw material availability; Can only implement the regenerative response under low pH (5.8-6.5) condition, advantages such as the absorbing activity of the high regenerative response speed of magnesium method desulfurization, high PH reaction solution, the separation of reaction generation sediment free settling are not embodied fully, mainly show:
Absorption system still is low pH slurries circulating system, equipment anticorrosion, wear-resisting and anti-blocking requirement height, and key equipments such as stirring in circulating pump, the tower, shower nozzle still need import, and the engineering equipment investment is big;
Receive the restriction of low pH absorption liquid absorption reaction activity and absorptive capacity, for reaching higher desulfuration efficiency, still need bigger liquid-gas ratio, flue gas is bigger in the pressure loss of absorption system, and power consumption and operating cost are bigger;
Regenerative response is to equipment requirements is high, power consumption is big, efficient is low in the tower.
The desulfurization product oxidation generates only 5-10% of magnesium sulfate concentration, and comprehensive utilization value is low, consumes a large amount of supplementing water simultaneously; Desulfurization product adopts the recovery system of roasting recovery magnesia technology huge, and investment and energy consumption are big;
Regenerative response is incomplete, and the magnesian utilization rate of medicament is low, has increased operating cost, has increased the difficulty of Treatment of Sludge;
For improving the reaction rate of regenerative response in the tower, need magnesia unslacked is digested to magnesium hydroxide, increased investment of devices and power, consumption of heat energy.
Summary of the invention
The sulfur removal technology of a kind of using external regenerative cycle magnesium sulfate method flue gas or waste gas, it comprises the following steps:
Flue gas or waste gas that step 1. will contain sulfur dioxide are introduced the absorption tower continuously; Absorb the sulfur dioxide in flue gas or the waste gas with the circulation of magnesium sulfite absorption liquid; Make the magnesium sulfite in the absorption liquid change into magnesium bisulfite, remove the sulfur dioxide in flue gas or the waste gas, its reaction is:
MgSO
3+SO
2+H
2O→Mg(HSO
3)
2 (1)
Reaction (1) is a fast response, and it is active under low liquid-gas ratio, to have possessed high absorption reaction.Absorption reaction is controlled by air film, reduces the absorption liquid temperature, and the pH value that improves absorption liquid helps reducing SO
2Equilibrium partial pressure, improve absorption efficiency.
Mg(HSO
3)
2+MgO→MgSO
3↓+H
2O (2)
Because the reaction product magnesium sulfite is the slightly soluble material; Its solubility is much larger than the solubility of calcium method calcium sulfite; The magnesium sulfite that regenerative response produces gets into liquid phase rapidly and combines to generate three water magnesium sulfite crystallizations with crystal seed; Avoided magnesium sulfite to influence further carrying out of regenerative response in the deposition of mgo surface, the reproduction speed of reaction (2) is far above the calcium method for this reason.
Step 3. is filtered the regenerated liquid of step 2 gained, reclaims the magnesium sulfite solid, and filtrating turns back to the absorption tower absorption that circulates, constantly with the sulfur dioxide removal in flue gas or the waste gas.
The above-mentioned using external regenerative cycle magnesium sulfate method flue gas or the sulfur removal technology of waste gas, the magnesium sulfite absorption liquid is solution or the suspension that comprises magnesium sulfite or magnesium sulfite and magnesium bisulfite in the described step 1.
The above-mentioned using external regenerative cycle magnesium sulfate method flue gas or the sulfur removal technology of waste gas, the pH=6-6.8 of absorption liquid at the bottom of the described absorption tower of step 2.
The above-mentioned using external regenerative cycle magnesium sulfate method flue gas or the sulfur removal technology of waste gas, the spray flux of the described absorption liquid of step 1 are 1-4 liter/mark cubic meter flue gas.In this liquid-gas ratio scope, the clearance of sulfur dioxide is 85-99.5%.
The above-mentioned using external regenerative cycle magnesium sulfate method flue gas or the sulfur removal technology of waste gas, the described magnesia slurries of step 2 are to contain magnesia or/and the slurries of magnesium hydroxide also can be directly to use magnesia solid regenerated.
The above-mentioned using external regenerative cycle magnesium sulfate method flue gas or the sulfur removal technology of waste gas, to distribute the outer regenerative system of part or all of entering tower be to distribute absorption liquid at the bottom of the tower of 25-100% to absorption liquid at the bottom of the described tower of step 2.
The above-mentioned using external regenerative cycle magnesium sulfate method flue gas or the sulfur removal technology of waste gas, the regenerative response time of the described regenerative process of step 2 needs 12-36 minute.
The above-mentioned using external regenerative cycle magnesium sulfate method flue gas or the sulfur removal technology of waste gas, the described regenerative process of step 2, its startup stage, through adding the crystallization water content and the particle diameter of its crystal of crystal seed control, the composition of crystal seed is three water magnesium sulfites.
The above-mentioned using external regenerative cycle magnesium sulfate method flue gas or the sulfur removal technology of waste gas, the pH of the filtrating after the described regeneration of step 3 is 7.2-8.5.
The above-mentioned using external regenerative cycle magnesium sulfate method flue gas or the sulfur removal technology of waste gas, the temperature of the described regeneration rear filtrate of step 3 is 38-48 ℃.
The above-mentioned using external regenerative cycle magnesium sulfate method flue gas or the sulfur removal technology of waste gas, the filtrating after the described regeneration of step 3 are clear liquid or solid-liquid mixing suspension, and the mass ratio of its solid content is 0-1.5%.Its liquid phase main component is the aqueous solution of magnesium sulfite and magnesium sulfate, and solid phase composition main component is magnesium sulfite, magnesia and/or magnesium hydroxide.Magnesium sulfate in the liquid phase be owing to the dioxygen oxidation that contains some in the flue gas magnesium sulfite form, be the side reaction in the course of reaction:
2MgSO
3+O
2→2MgSO
4 (3)
The MgSO that reaction (3) generates
4Influence the absorbing activity of absorption liquid, through its concentration in circulating system of draining control.
The above-mentioned using external regenerative cycle magnesium sulfate method flue gas or the sulfur removal technology of waste gas; Described absorption tower comprises the upper and lower two-layer spraying layer that is positioned at the absorption tower; Absorption liquid after the regeneration preferentially gets into the upper strata spray, and the pH value of upper strata spray absorption liquid is more than or equal to the pH value of lower floor's spray absorption liquid.
The above-mentioned using external regenerative cycle magnesium sulfate method flue gas or the sulfur removal technology of waste gas; Before step 1, setting up procedure can be arranged: the flue gas or the waste gas that will contain sulfur dioxide are introduced the absorption tower continuously; Be lower than 0.5% magnesium hydroxide slurry with solid content in the absorption system absorption that circulates; Remove the sulfur dioxide in flue gas or the waste gas, accomplish start-up course to absorption liquid pH≤6 backs, absorption liquid gets into the external regeneration system and regenerates.Following chemical absorbing reaction takes place in the absorption tower during this time:
Mg(OH)
2+SO
2→MgSO
3 (4)
MgSO
3+SO
2+H
2O→Mg(HSO
3)
2 (5)
Reaction (4) (5) are the main chemical reaction that absorbs, and the startup incipient stage is mainly reacted (4), and this reaction is long response time, and absorption process is controlled by liquid film, and absorption efficiency is extremely low; Along with the carrying out of reaction (4), liquid phase MgSO3 concentration constantly increases, and absorption process is mainly reacted (5), and this reaction is fast response, and absorption efficiency significantly improves; Along with constantly carrying out of absorption process, liquid phase Mg (HSO3) 2 content increase, and pH value of solution reduces, and behind pH≤6, absorption efficiency significantly descends, and absorption liquid at the bottom of the absorption tower is got into the outer regenerative system of tower, regeneration magnesium sulfite absorption liquid.
Advantage of the present invention is in particular in:
The outer regeneration technology of absorption liquid tower; The pH of regenerative response terminal point and the conversion ratio of medicament have been improved; Reduce the temperature of absorption liquid, made absorption liquid possess the characteristics of high pH (7.2-8.5), low temperature (38-48 ℃), high absorptive capacity, effectively improved the absorbing activity of absorption liquid;
The absorption liquid of high absorbing activity has reduced the liquid-gas ratio of absorption system, has reduced the pressure loss of flue gas in desulphurization system simultaneously.(under the situation that reaches identical removal efficient, liquid-gas ratio of the present invention and air-channel system crushing be merely conventional oxidation magnesium method 1/2 and 3/5), effectively reduce operating cost;
Because absorption system is the low-solid content absorption liquid circulating system of high pH; Equipment and pipeline anticorrosion antiwear require to reduce; Avoided the import of key equipments such as desulfuration recycle pump, shower nozzle, the interior stirring of tower, the high reaction activity of absorption liquid has reduced the volume on absorption tower simultaneously, and equipment investment significantly reduces;
The outer regenerative response of tower has further improved regenerative response speed and efficient; Induced crystallization technology makes regeneration product magnesium sulfite crystal formation good, has created condition for follow-up efficient Separation of Solid and Liquid, and the equipment scale of external regeneration system is little;
Power consumption significantly reduces; Improve constantly under the situation in present promotion energy-saving and emission-reduction and rate for incorporation into the power network; The advantage of the present invention aspect society, economy, environmental benefit is obvious day by day; In non-electricity or thermoelectric enterprise, because its electricity rates and rate for incorporation into the power network all are higher than electricity power enterprise, its economic advantages are obvious further simultaneously;
The solidliquid mixture that Separation of Solid and Liquid produces after mud concentrates, need not to carry out press filtration and handles, and its content of magnesium has reached 5-8%, if with its oxidation, the magnesium sulfate concentration of generation approaches the saturated concentration of magnesium sulfate, produces magnesium sulfate for comprehensive utilization and has created condition;
The magnesian utilization rate of desulfurizing agent improves 5-10% than prior art.Magnesia slurries (solid) are directly participated in regenerative response, need not magnesian digestion process; Material consumption, energy consumption, the water consumption of digestion facility and digestion process have been reduced;
Employing equipment is conventional homemade common apparatus, and the present invention uses on medium and small boiler flue gas desulfurization still has good cost performance;
Increased the floor space of regenerative system than magnesium oxide method, but because the reclaim equiment scale is less, the regenerative system floor space is in the acceptable scope of electric power enterprise.Simultaneously, regenerative system can be arranged with the absorption system branch, is convenient to the floor plan of project and the desulfurization transformation of old facility.
Description of drawings
Fig. 1 is a process flow diagram of the present invention, and wherein: 1 is desulfuration absorbing tower, and 2 is the liquid storage section, and 3 are lower floor's spray; 4 are the upper strata spray, and 5 is demister, and 6 is the absorption liquid storage tank; 7 are the regeneration liquid bath, and 8 is static mixer, and 9 is magnesia slurry batch tank; 10 is regeneration reactor, and 11 is sedimentation basin, and 12 is filter press.
The specific embodiment
Embodiment
Shown in process chart: through the boiler sulfur-containing smoke gas of dust removal process, send into desulfuration absorbing tower 1, absorb desulfurization with the absorption liquid counter current contacting of lower floor's spray 3 and upper strata spray 4 ejections by air-introduced machine, through demister 5 demists after the chimney emptying.Liquid storage section absorption liquid, partially absorbs liquid and proceeds the desulfurization absorption by circulating pump through lower floor's spray that pipeline 14 pumps in the absorption tower from flowing into the absorption liquid storage tank tower outside through pipeline 13 at the bottom of the tower, partially absorbs liquid and is reproduced pump and pumps into static mixer 8 through pipeline 15.Magnesia powder as desulfurizing agent; Sending into magnesia slurry batch tank 9 from the magnesia storage tank mixes with fresh water (FW) and joins slurry; The magnesia slurry of configuration pumps into static mixer 8 by mashing pump through pipeline 16 and carries out high efficient mixed with the absorption liquid that gets into, and mixed suspension gets into regeneration reactor 10 through pipeline 18 and carries out regenerative response; The absorption liquid of accomplishing regenerative response carries out the separation of solid-liquid body through pipeline 19 from flowing into sedimentation basin 11, and sediment is transported outward comprehensive utilization or sanitary landfills by sludge pump after pipeline 21 pumps into the filter press press filtration.From flowing into regenerated liquid groove 7, regeneration liquid bath 7 links to each other through subsurface pipeline 22 with absorption liquid storage tank 6 through pipeline 20 for the upper strata suspension of sedimentation basin or clear liquid, to keep the level balance of regeneration liquid bath 7 and absorption liquid storage tank 6.Absorption liquid in the regeneration liquid bath 7 carries out the desulfurization absorption by spray pump through the upper strata spray that pipeline 17 pumps in the absorption tower.According to regeneration liquid measure big I be provided with a plurality of parallel connections or series connection static mixer and regeneration reactor.
We utilize one 75 of certain thermoelectric enterprise to steam a ton/hour coal-fired fluidized bed boiler and are provided with experimental provision of the present invention by above-mentioned technological process; Boiler steady-state operation parameter is: exhaust gas volumn 100,000 mark cubic meters/hour; 135 ℃ of desulfurizer gas approach temperature, SO 2 from fume concentration 1260-1450 milligram/mark cubic meter.Absorption system and regenerative system apart arrangement, 120 square metres of regenerative system floor spaces.Desulphurization system is provided with as follows:
Absorption system: absorption tower Φ 2800 * 15000; Adopt spray column, two-layer spray; Upper and lower layer spray provides absorption liquid respectively by two circulating pumps; The upper strata spray adopts the high pH absorption liquid in the regeneration liquid bath, and lower floor's spray adopts the low pH absorption liquid in the circulation liquid bath, and pump flow passes through VFC.Two-layer corrugated plating demister, resistance 200Pa are established in the top, absorption tower; Establish the liquid storage section at the bottom of the absorption tower, 2 meters of height; Each 20 cubic metres of regeneration liquid bath, absorption liquid storage tanks, pipeline links to each other to keep level balance under the two tank liquor faces.
Regenerative system: low pH absorption liquid pumps into regenerative system by regenerative pump, through regenerative pump is implemented its regenerant flow of VFC; 10 cubic metres of magnesia slurry batch tank dischargeable capacitys; Stirring is set, magnesia concentration of slurry 20%, configuration magnesia slurries do not carry out slaking; Adopt measuring pump that the magnesia slush pump is gone into static blender, regenerative process added the magnesia slurry by magnesium sulphur than 1.08: 1; Regeneration reactor is made up of the stirred tank of four parallel connections, 20 cubic metres of every stirred tank dischargeable capacitys, and the cooling heat transferring face is established in the stirred tank outside, through being arranged on the use number of the valve control stirred tank before the stirred tank, thereby regulates the regenerative response time of staying; Solid-liquid separation system adopts inclined-plate clarifying basin, 50 square metres of sedimentation basin surface areas.Mud adopts the plate and frame filter press drying and other treatment.
Under flue gas steady-state operation parameter condition; According to the form below content adjustment liquid-gas ratio, reproduction ratio and the regeneration time of staying; After treating regenerative system stable operation, measure the temperature and the solid content of desulfuration efficiency, desulphurization system crushing, regenerative response pH variation, regenerative system water outlet, test data shows; Under the condition of following examples, desulphurization system all can reach satisfactory absorption efficiency.Adopt operation and the online detection of flue gas of 7 continuous half a year of embodiment to show: system's desulfuration efficiency maintains more than 95% all the time, stable equipment operation, and discovery has fouling and burn into wear phenomenon.
Claims (8)
1. the sulfur removal technology of using external regenerative cycle magnesium sulfate method flue gas or waste gas is characterized in that it comprises the following steps:
Flue gas or waste gas that step 1. will contain sulfur dioxide are introduced the absorption tower continuously; Absorb the sulfur dioxide in flue gas or the waste gas with the circulation of magnesium sulfite absorption liquid; Make the magnesium sulfite in the absorption liquid change into magnesium bisulfite, remove the sulfur dioxide in flue gas or the waste gas
Step 2. with the absorption tower at the bottom of absorption liquid distribute the outer regenerative system of part or all of entering tower, regenerate with the magnesia slurry reaction,
Step 3. is filtered the regenerated liquid of step 2 gained; Reclaim the magnesium sulfite solid, filtrating turns back to the absorption tower absorption that circulates, constantly with the sulfur dioxide removal in flue gas or the waste gas; Filtrating after the described regeneration is clear liquid or solid-liquid mixing suspension; The mass ratio of its solid content is 0-1.5%, and its liquid phase main component is the aqueous solution of magnesium sulfite and magnesium sulfate, and the solid phase main component is magnesium sulfite, magnesia and/or magnesium hydroxide.
2. the sulfur removal technology of using external regenerative cycle magnesium sulfate method flue gas according to claim 1 or waste gas is characterized in that: the pH=6-6.8 of absorption liquid at the bottom of the described absorption tower of step 2.
3. the sulfur removal technology of using external regenerative cycle magnesium sulfate method flue gas according to claim 1 or waste gas is characterized in that: the described magnesia slurries of step 2 are to contain magnesia or/and the slurries of magnesium hydroxide, or directly use magnesia solid regenerated.
4. the sulfur removal technology of using external regenerative cycle magnesium sulfate method flue gas according to claim 1 or waste gas is characterized in that: to distribute the outer regenerative system of part or all of entering tower be to distribute absorption liquid at the bottom of the tower of 25-100% to absorption liquid at the bottom of the described tower of step 2.
5. the sulfur removal technology of using external regenerative cycle magnesium sulfate method flue gas according to claim 1 or waste gas; It is characterized in that: the described regenerative process of step 2; Its startup stage, through adding the crystallization water content and the particle diameter of its crystal of crystal seed control, the composition of crystal seed is three water magnesium sulfites.
6. the sulfur removal technology of using external regenerative cycle magnesium sulfate method flue gas according to claim 1 or waste gas is characterized in that: the pH of the filtrating after the described regeneration of step 3 is 7.2-8.5.
7. the sulfur removal technology of using external regenerative cycle magnesium sulfate method flue gas according to claim 1 or waste gas; It is characterized in that: described absorption tower comprises the upper and lower two-layer spraying layer that is positioned at the absorption tower; Absorption liquid after the regeneration preferentially gets into the upper strata spray, and the pH value of upper strata spray absorption liquid is more than or equal to the pH value of lower floor's spray absorption liquid.
8. the sulfur removal technology of using external regenerative cycle magnesium sulfate method flue gas according to claim 1 or waste gas; It is characterized in that: before step 1, setting up procedure is arranged: the flue gas or the waste gas that will contain sulfur dioxide are introduced the absorption tower continuously; Be lower than 0.5% magnesium hydroxide slurry with solid content in the absorption system absorption that circulates; Remove the sulfur dioxide in flue gas or the waste gas, accomplish start-up course to absorption liquid pH≤6 backs, absorption liquid gets into the external regeneration system and regenerates.
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| CN113082962B (en) * | 2021-04-21 | 2023-01-17 | 江苏联慧资源环境科技有限公司 | Secondary mixed magnesium method flue gas desulfurization process and device |
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