CN103818884A - Process for decomposing gypsum through spraying and fluidizing - Google Patents
Process for decomposing gypsum through spraying and fluidizing Download PDFInfo
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Abstract
The invention relates to the technical field of fluidized decomposition and calcination of gypsum, and particularly discloses a process for producing sulfuric acid by spraying, fluidizing, decomposing and calcining gypsum efficiently. The process comprises the following steps: gasifying brimstone; preheating raw gypsum; spraying, fluidizing and decomposing gypsum to prepare calcium sulfide and sulfur dioxide; preparing sulfur dioxide by calcining and decomposing the prepared calcium sulfide and heated gypsum; preparing sulfuric acid by treating the tail gas. Through the adoption of spraying and fluidizing technology, out-kiln decomposition of gypsum during acid making is realized; the calcium sulfide can be prepared efficiently with low cost; then the calcium sulfide and the preheated gypsum are calcined together for decomposition to prepare the sulfur dioxide. Therefore, the process is absolutely an excellent process for industrialized continuous production, is high in economic benefits and energy utilization ratio.
Description
Technical field
The invention belongs to gypsum relieving haperacidity technical field, particularly a kind of terra alba fluidization precalcining technique, the inventive method can also be prepared sulfuric acid simultaneously.
Background technology
Along with the high speed development day by day of China's economy, a large amount of Industrial Solid Waste gypsum are badly in need of follow-up digestion process:
1, phosphogypsum is the byproduct of sulfuric acid process phosphoric acid extraction, 1 ton of ammonium phosphate product of every production, approximately produce 2.5 tons of phosphogypsums, along with China's phosphorus ammonium industry fast development, the amount of byproduct phosphogypsum is increasing, the stacking of phosphogypsum has not only taken a large amount of land resources, and also due to wind erosion, weathering atmosphere pollution, cienega and soil, and the cost of erection of ardealite storage yard is also quite expensive.
2, the salt slag that salt industry produces, long-term thrown aside gully pile up like a mountain, or enters river in overflow stage, causes environmental pollution to a certain degree and the social danger of appropriation of land.
3, along with the increasingly stringent of environment protection, the desulfurization slag that the industry such as thermal power generation produces is more and more, and a large amount of heaps are abandoned.
4, Gypsum Mine exploitation usually throw aside a large amount of anhydrite need not.
The comprehensive regulation of phosphogypsum, desulfurated plaster, salt gypsum, anhydrite etc. Industrial Solid Waste has become our problem in the urgent need to address of country.
One of effective way that phosphogypsum producing sulfuric acid and jointly cement processed is gypsum industry waste reside comprehensive utilization, China's tackling key problem that begins one's study from the sixties, has built many covers Industrial demonstration device the nineties, makes phosphoric acid-phosphogypsum-sulfuric acid realize organic cycle.The technique of phosphogypsum producing sulfuric acid and jointly cement processed comprises the following steps: six processes such as material homogenizer, drying and dewatering, raw material preparation, grog burn till, kiln gas relieving haperacidity and cement grind.
Phosphogypsum producing sulfuric acid and jointly cement processed can effectively utilize byproduct phosphogypsum to make sulfuric acid, and obtains cement products, turns waste into wealth, and has good economic benefit and environmental benefit.But there is following problem in traditional Discussion on technology for production of SA with joint product cement from phosphogypsum: adopt coke to do reductive agent decomposing gypsum, cost of material is high, and then causes product cost high; In grog sintering process, adopt decomposing and calcining technology in the hollow kiln kiln falling behind in cement production process, energy consumption is high, desulfurization degree is low; Decomposing and calcining step complete operation difficulty in hollow kiln is large, and balling ring formation is serious, and unit service factor is low, and unit production capacity is low.
Chinese patent CN101708826A has announced a kind of method of sulphur reducing and decomposing phosphogypsum.The method is: phosphogypsum is put into reactor and under inert atmosphere, be warming up to 500～900 ℃ of preheatings 10～30 minutes, then passing into mole fraction and be 10～50% gaseous state sulphur and phosphogypsum carries out after reduction reaction 1～2h, by after the abrasive lapping of gained sulfurated lime again with phosphogypsum in molar ratio 1～1.5:3 mix, roasting 0.5～3h at 1000 ℃～1400 ℃ in non-oxidizing atmosphere, the SO producing
2gas is as the raw material of producing sulfuric acid, and gained solid slag can be used as the raw material of manufacture of cement.More than the rate of decomposition of phosphogypsum can reach 98wt%, more than desulfurization degree can reach 95wt%.Aforesaid method is only experimental technique; because be not tandem reaction sequence; cannot directly carry out suitability for industrialized production, if the method will realize suitability for industrialized production, need to there is the thermal equilibrium of solution the first step reactive system and the inertia of the first step reaction gas sulphur protection problem of economy.Therefore the method still can not be carried out suitability for industrialized production.
Summary of the invention
The object of the invention is to overcome existing above-mentioned deficiency in prior art, provide a kind of and can realize that industrialization is produced continuously, operation easier is low, the spouted fluidized precalcining process for preparing sulfuric acid of high gypsum rate of decomposition.
The spouted fluidized decomposition technique of gypsum provided by the invention, is characterized in that, comprises the following steps:
(1), sulphur is heated to 120 ℃～150 ℃ in sulfur melting groove, obtain Molten sulphur.
(2), Molten sulphur is through liquid sulfur pump feeding molten sulfur gasification burner, the waste heat tail gas of discharging with rotary kiln tail carries out heat exchange, makes Molten sulphur gasification be warming up to 450 ℃～750 ℃, the waste heat tail gas after heat exchange enters secondary cyclone preheater.
(3), in feed bin mean particle size be 1 μ m～200 μ m gypsum raw meal powder in the waste heat tail gas mark condition volume ratio ratio that is 1:4000～10000, carry out heat exchange through feeding machine feeding one-level cyclone preheater and waste heat tail gas, be warming up to 50 ℃～400 ℃, the raw material of process one-level cyclone preheater preheating enter secondary cyclone preheater and waste heat tail gas carries out heat exchange, be warming up to 200 ℃～700 ℃, enter together with the solid materials that spouted fluidized bed, a part discharge with spouted fluidized bed and enter rotary kiln through a raw material part for secondary cyclone preheater preheating; The waste heat tail gas of discharging after the heat exchange of secondary cyclone preheater enters the heat exchange of one-level cyclone preheater.
Described volume ratio refers to the gas volume ratio under solid raw meal powder volume and waste heat tail gas standard state.
Regulate according to the response behaviour of each material in device the ratio that enters spouted fluidized bed and enter rotary kiln through the raw material of secondary preheating, make device reaction abundant.
(4) air that, fuel blasts with gas blower in hotblast stove is fully burning after mixing by air excess 5%～15%, the sulfur gas that the hot flue gas producing and molten sulfur vapourizing furnace come by volume 0.2～10:1 is mixed, consume the remaining oxygen in hot flue gas, form the mixed flue gas containing sulfur vapor of 600 ℃～1100 ℃, mixed flue gas enters spouted fluidized bed.
(5), in spouted fluidized bed, carry out spouted fluidized heat exchange decomposition reaction with the mixed flue gas containing sulfur vapor through the raw material of secondary preheating at 500 ℃～1000 ℃, the solid materials after decomposition reaction is discharged through overflow port; Fluidized-bed tail gas enters tornado dust collector, and the powder under separating returns to spouted fluidized bed.
(6), the solid materials of the step 5 gained pre-plaster of paris raw meal powder with step 3 mixes, and controls CaS and CaSO in mixture
4mol ratio is that 1.0～1.5:3 sends into rotary kiln, at 800 ℃～1300 ℃, reacts 0.5～5 hour, obtains containing the tail gas of sulfurous gas and the solid slag containing calcium oxide.
Further, the tail gas that spouted fluidized bed is discharged, through tornado dust collector purification, again through except after sulfur vapor, is sent to sulfuric acid apparatus, for the preparation of sulfuric acid.Preferably, the tail gas that one-level cyclone preheater is discharged is sent to sulfuric acid apparatus, for the preparation of sulfuric acid.
The present invention adopts the mixed gas of sulfur vapor and hot flue gas as fluidized-bed fluidisation carrier and reaction raw materials, react with the gypsum raw material of the process thermal pretreatment of mean particle size 1 μ m～200 μ m, material contact area is more abundant more greatly, the dividing potential drop ratio of sulfur vapor is higher, speed of reaction is fast, thermo-efficiency is high, and FU volume production is high, and material decomposes more thoroughly and be more easy to control.
The spouted fluidized decomposition technique of gypsum as mentioned above, it is characterized in that, in step (4), the fluidized wind air inlet of spouted fluidized bed is tangential admission, effectively short feeding gas mixes, the spouted wind of spouted fluidized bed is Rafael nozzle, effectively improve the cycling rate of material in spouted stove, improve gypsum meal calcining rate.
The spouted fluidized decomposition technique of gypsum, is characterized in that as mentioned above, and in step (4), described fuel is at least one in Sweet natural gas, coal gas, liquefied petroleum gas (LPG), hard coal, bituminous coal or high sulphur coal.Preferably, described fuel is high sulphur coal.High sulphur coal, as other industrial inferior fuels, still can effectively improve sulphuric acid output and reduce production costs for this technique.
Preferably, described fuel blasts the hot flue gas of oxygen-rich air burning generation of oxygen level 25-50% in hotblast stove through gas blower.Oxygen-rich air burning can provide more heat, effectively maintains the heat balance of spouted fluidized bed reaction, further reduces product hear rate, increase the abundant rate of reaction, improve SO2 concentration in tail gas, reduce side reaction, improve the purity of target product, reduce products production cost.
The spouted fluidized decomposition technique of gypsum, is characterized in that as mentioned above, and described gypsum is at least one in phosphogypsum, desulfurated plaster, salt gypsum, fluorgypsum, citric acid gypsum, nickel gypsum, titanium dioxide by-product gypsum, the plaster of paris, natural anhydrite.
The described tail gas containing sulfurous gas of step (6) as mentioned above, the percent by volume of sulfurous gas is 5%～25%, can be used for preparing sulfuric acid.
The described solid slag containing calcium oxide of step (6) as mentioned above, the mass percent of calcium oxide is 15%～75%.
The spouted fluidized decomposition technique of gypsum as above, gypsum raw meal powder is continuous dosing, the spouted fluidized decomposing and calcining system of gypsum raw meal powder is continuous flow procedure, can improve device output, production control cost, is conducive to the industrialization of this technique.
The spouted fluidized decomposition technique of gypsum as above, liquid sulfur pump is arranged in sulfur melting groove, reduces calorific loss.
The present invention compared with prior art, has following notable feature and beneficial effect:
1. in the spouted fluidized decomposition technique of gypsum, sulphur heating is obtained to Molten sulphur, can evenly enter into vapourizing furnace, make Production Flow Chart steady.
2. owing to containing SO
2tail gas must carry out cooling before sulfuric acid processed, both can cooled exhaust gas after the tail gas heat exchange out of gypsum raw meal powder and Molten sulphur and rotary kiln tail, can utilize again waste heat to make Molten sulphur gasification and the preheating of gypsum raw meal powder, not only realize technique object but also save energy, reduction energy consumption.
3. after adopting fuel to burn in hotblast stove, directly mix with High Temperature Gas sulphur again; both can carry out direct heating to gas sulphur; reduce the calorific loss in heat transfer process; can eliminate again and blast oxygen superfluous in hot blast furnace air, make the process gas that enters spouted fluidized bed participation decomposition reaction form non-oxide protective atmosphere.
4. adopt spouted fluidized bed as decomposition reactor, and make fluidized wind along the undercutting of fluidized-bed cone to entering, add the contact area of atmospheric sulfer and terra alba, make gas sulphur and terra alba raw material under fluidized state, carry out abundant heat exchange, enhance heat transfer mass transfer effect, accelerate speed of reaction, effectively improve material rate of decomposition, reduce energy consumption; The decomposition of terra alba raw material is carried out outward at rotary kiln, has reduced rotary kiln thermal load, effectively improves gypsum sulphuric acid plant unit production capacity; Terra alba raw material decompose and calcining is separately carried out, and effectively avoid rotary kiln balling, ring formation, reduce operation easier, realize industrialization and produce continuously.
Accompanying drawing explanation:
Fig. 1 is process flow sheet of the present invention
Mark in figure: 1-gas blower, 2-hotblast stove, 3-spouted fluidized bed, 4-tornado dust collector, 5-feed bin, 6-feeding machine, 7-one-level cyclone preheater, 8-secondary cyclone preheater, 9-molten sulfur gasification burner, 10-rotary kiln, 11-sulfur melting groove, 12-liquid sulfur pump.
Embodiment
Below in conjunction with test example and embodiment, the present invention is described in further detail.But this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following embodiment, all technology realizing based on content of the present invention all belong to scope of the present invention.Per-cent not specified in the present invention is all weight percentage.
Solid sulfur obtains Molten sulphur through saturated vapor indirect heat exchange sulfur melting groove 11 is interior; Molten sulphur feeds molten sulfur gasification burner 9 through liquid sulfur pump 12 sulfur melting groove 11 is interior, and the waste heat tail gas of discharging with rotary kiln 10 kiln tails carries out indirect heat exchange, makes Molten sulphur gasification for the sulfur vapor wind furnace 2 that reduces phlegm and internal heat, and waste heat tail gas enters secondary cyclone preheater 8; Gypsum raw meal powder in feed bin 5 feeds one-level cyclone preheater 7 through feeding machine 6, raw material through one-level preheating enter secondary cyclone preheater 8, enter together with the solid materials that spouted fluidized bed 3, a part discharge with spouted fluidized bed and enter rotary kiln through a raw material part for secondary preheating; The air that fuel blasts with gas blower 1 in hotblast stove 2 or oxygen-rich air burning form hot flue gas, the gas sulphur of molten sulfur vapourizing furnace 9 and hot flue gas are mixed, consume the superfluous oxygen in hot flue gas, obtain the gas mixture of gas sulphur and flue gas, mixed air enters spouted fluidized bed 3; Preheated raw meal in spouted fluidized bed 3 with gas mixture direct contact heat transfer, carry out spouted fluidized decomposition reaction, tail gas enters tornado dust collector 4, the powder under tornado dust collector 4 separate returns to spouted fluidized bed 3, the solid materials after decomposition reaction is discharged through overflow port; Solid materials is allocated the appropriate raw meal powder through secondary preheating into and is sent into rotary kiln 10 and calcine, and obtains containing the tail gas of sulfurous gas with containing the solid slag of calcium oxide; The tail gas clean-up of tornado dust collector 4 is except sending to sulfuric acid apparatus sulfuric acid processed with together with the tail gas of one-level cyclone preheater 7 after sulfur vapor.
In following examples, terra alba raw material are continuous dosing, and the spouted fluidized decomposing and calcining system of terra alba is continuous flow procedure.
Embodiment 1
1: half water phosphogypsum powder of raw material.Table 1 is its chemical composition.
Raw material 2: sulphur (purity 99.8wt%)
Table 1 half water phosphogypsum powder chemical composition
Fuel: Sweet natural gas.Table 2 is its chemical composition.
Table 2 natural gas chemistry composition
| Component | CH 4 | C 2H 6 | C 3H 8 | CO 2 | N 2 |
| Content/vol% | 97.23 | 0.18 | 0.07 | 1.3 | 1.22 |
Solid sulfur is in the interior Molten sulphur that obtains 150 ℃ through saturated vapor indirect heat exchange of sulfur melting groove 11; Molten sulphur feeds molten sulfur vapourizing furnace 9 through liquid sulfur pump 12 sulfur melting groove 11 is interior, and the waste heat tail gas of discharging with rotary kiln 10 kiln tails carries out indirect heat exchange, and making Molten sulphur gasification is the sulfur vapor of the 550 ℃ wind furnace 2 that reduces phlegm and internal heat, and waste heat tail gas enters secondary cyclone preheater 8; The interior mean particle size of feed bin 5 be 50 μ m gypsum raw meal powder by with mixed flue gas mark condition volume ratio be that 1:6000 feeds one-level cyclone preheater 7 through feeding machine 6, be warming up to 300 ℃, raw material through one-level preheating enter secondary cyclone preheater 8, be warming up to 500 ℃, enter together with the solid materials that spouted fluidized bed 3, a part discharge with spouted fluidized bed and enter rotary kiln through a raw material part for secondary preheating; Fuel forms hot flue gas with the air that gas blower 1 blasts by air excess 10% mixed firing in hotblast stove 2, the gas sulphur of molten sulfur vapourizing furnace 9 and hot flue gas by volume 1:5 are mixed, consume the superfluous oxygen in hot flue gas, form the mixed flue gas of 750 ℃, mixed air enters spouted fluidized bed 3; Preheated raw meal is carried out spouted fluidized heat exchange decomposition reaction with the mixed flue gas of gassiness sulphur at 600 ℃ in spouted fluidized bed 3; Tail gas enters tornado dust collector 4, and the powder under tornado dust collector 4 separate returns to spouted fluidized bed 3, and the solid materials after decomposition reaction is discharged through overflow port; Solid materials mixes with the gypsum raw meal powder of process secondary preheating, controls CaS and CaSO in mixture
4mol ratio 1.2:3 sends into rotary kiln 10 and calcines, and at 1200 ℃, reacts 2h, obtains containing the tail gas that sulfurous gas volume fraction is 15% and the solid slag that is 53% containing calcium oxide massfraction.The tail gas clean-up of tornado dust collector 4 is except sending to sulfuric acid apparatus sulfuric acid processed with together with the tail gas of one-level cyclone preheater 7 after sulfur vapor.
Raw material 1: desulfurization gypsum powder.Table 1 is its chemical composition.
Raw material 2: sulphur (purity 99.8wt%)
Table 3 desulfurization gypsum powder chemical composition
Fuel: hard coal.Table 4 is its technical analysis.
The technical analysis of table 4 hard coal
| Component | Fixed carbon | Volatile matter | Ash content | Moisture |
| Content/wt% | 70.0 | 4.3 | 20.5 | 5.2 |
Solid sulfur is in the interior Molten sulphur that obtains 130 ℃ through saturated vapor indirect heat exchange of sulfur melting groove 11; Molten sulphur feeds molten sulfur vapourizing furnace 9 through liquid sulfur pump 12 sulfur melting groove 11 is interior, and the waste heat tail gas of discharging with rotary kiln 10 kiln tails carries out indirect heat exchange, and making Molten sulphur gasification is the sulfur vapor of the 450 ℃ wind furnace 2 that reduces phlegm and internal heat, and waste heat tail gas enters secondary cyclone preheater 8; The interior mean particle size of feed bin 5 be 120 μ m gypsum raw meal powder by with mixed flue gas mark condition volume ratio be that 1:4000 feeds one-level cyclone preheater 7 through feeding machine 6, be warming up to 400 ℃, raw material through one-level preheating enter secondary cyclone preheater 8, be warming up to 700 ℃, enter together with the solid materials that spouted fluidized bed 3, a part discharge with spouted fluidized bed and enter rotary kiln through a raw material part for secondary preheating; Fuel forms hot flue gas with the air that gas blower 1 blasts by air excess 5% mixed firing in hotblast stove 2, the gas sulphur of molten sulfur vapourizing furnace 9 and hot flue gas by volume 1:10 are mixed, consume the superfluous oxygen in hot flue gas, form the mixed flue gas of 1000 ℃, mixed air enters spouted fluidized bed 3; Preheated raw meal is carried out spouted fluidized heat exchange decomposition reaction with the mixed flue gas of gassiness sulphur at 900 ℃ in spouted fluidized bed 3; Tail gas enters tornado dust collector 4, and the powder under tornado dust collector 4 separate returns to spouted fluidized bed 3, and the solid materials after decomposition reaction is discharged through overflow port; Solid materials mixes with the gypsum raw meal powder of process secondary preheating, controls CaS and CaSO in mixture
4mol ratio 1.1:3 sends into rotary kiln 10 and calcines, and at 1000 ℃, reacts 3h, obtains containing the tail gas that sulfurous gas volume fraction is 10% and the solid slag that is 42% containing calcium oxide massfraction.The tail gas clean-up of tornado dust collector 4 is except sending to sulfuric acid apparatus sulfuric acid processed with together with the tail gas of one-level cyclone preheater 7 after sulfur vapor.
Embodiment 3
Raw material 1: salt terra alba.Table 5 is its chemical composition.
Raw material 2: sulphur (purity 99.8wt%)
Table 5 salt terra alba chemical composition
Fuel: bituminous coal.Table 6 is its technical analysis.
The technical analysis of table 6 bituminous coal
| Component | Fixed carbon | Volatile matter | Ash content | Moisture |
| Content/wt% | 56.0 | 20.6 | 17.8 | 5.6 |
Solid sulfur is in the interior Molten sulphur that obtains 130 ℃ through saturated vapor indirect heat exchange of sulfur melting groove 11; Molten sulphur feeds molten sulfur vapourizing furnace 9 through liquid sulfur pump 12 sulfur melting groove 11 is interior, and the waste heat tail gas of discharging with rotary kiln 10 kiln tails carries out indirect heat exchange, and making Molten sulphur gasification is the sulfur vapor of the 550 ℃ wind furnace 2 that reduces phlegm and internal heat, and waste heat tail gas enters secondary cyclone preheater 8; The interior mean particle size of feed bin 5 be 200 μ m gypsum raw meal powder by with mixed flue gas mark condition volume ratio be that 1:7000 feeds one-level cyclone preheater 7 through feeding machine 6, be warming up to 200 ℃, raw material through one-level preheating enter secondary cyclone preheater 8, be warming up to 400 ℃, enter together with the solid materials that spouted fluidized bed 3, a part discharge with spouted fluidized bed and enter rotary kiln through a raw material part for secondary preheating; Fuel forms hot flue gas with the air that gas blower 1 blasts by air excess 15% mixed firing in hotblast stove 2, the gas sulphur of molten sulfur vapourizing furnace 9 and hot flue gas by volume 1:8 are mixed, consume the superfluous oxygen in hot flue gas, form the mixed flue gas of 900 ℃, mixed air enters spouted fluidized bed 3; Preheated raw meal is carried out spouted fluidized heat exchange decomposition reaction with the mixed flue gas of gassiness sulphur at 700 ℃ in spouted fluidized bed 3; Tail gas enters tornado dust collector 4, and the powder under tornado dust collector 4 separate returns to spouted fluidized bed 3, and the solid materials after decomposition reaction is discharged through overflow port; Solid materials mixes with the gypsum raw meal powder of process secondary preheating, controls CaS and CaSO in mixture
4mol ratio 1.0:3 sends into rotary kiln 10 and calcines, and at 800 ℃, reacts 5h, obtains containing the tail gas that sulfurous gas volume fraction is 5% and the solid slag that is 15% containing calcium oxide massfraction.The tail gas clean-up of tornado dust collector 4 is except sending to sulfuric acid apparatus sulfuric acid processed with together with the tail gas of one-level cyclone preheater 7 after sulfur vapor.
Raw material 1: fluorine gypsum powder.Table 7 is its chemical composition.
Raw material 2: sulphur (purity 99.8wt%)
Table 7 fluorine gypsum powder chemical composition
Fuel: high sulphur coal.Table 8 is its technical analysis.
The technical analysis of table 8 high sulphur coal
| Component | Fixed carbon | Volatile matter | Ash content | Moisture |
| Content/wt% | 57.8 | 24.6 | 13.8 | 3.8 |
Solid sulfur is in the interior Molten sulphur that obtains 120 ℃ through saturated vapor indirect heat exchange of sulfur melting groove 11; Molten sulphur feeds molten sulfur vapourizing furnace 9 through liquid sulfur pump 12 sulfur melting groove 11 is interior, and the waste heat tail gas of discharging with rotary kiln 10 kiln tails carries out indirect heat exchange, and making Molten sulphur gasification is the sulfur vapor of the 750 ℃ wind furnace 2 that reduces phlegm and internal heat, and waste heat tail gas enters secondary cyclone preheater 8; The interior mean particle size of feed bin 5 be 10 μ m gypsum raw meal powder by with mixed flue gas mark condition volume ratio be that 1:5000 feeds one-level cyclone preheater 7 through feeding machine 6, be warming up to 50 ℃, raw material through one-level preheating enter secondary cyclone preheater 8, be warming up to 200 ℃, enter together with the solid materials that spouted fluidized bed 3, a part discharge with spouted fluidized bed and enter rotary kiln through a raw material part for secondary preheating; Fuel forms hot flue gas with the air that gas blower 1 blasts by air excess 8% mixed firing in hotblast stove 2, the gas sulphur of molten sulfur vapourizing furnace 9 and hot flue gas by volume 1:1 are mixed, consume the superfluous oxygen in hot flue gas, form the mixed flue gas of 650 ℃, mixed air enters spouted fluidized bed 3; Preheated raw meal is carried out spouted fluidized heat exchange decomposition reaction with the mixed flue gas of gassiness sulphur at 500 ℃ in spouted fluidized bed 3; Tail gas enters tornado dust collector 4, and the powder under tornado dust collector 4 separate returns to spouted fluidized bed 3, and the solid materials after decomposition reaction is discharged through overflow port; Solid materials mixes with the gypsum raw meal powder of process secondary preheating, controls CaS and CaSO in mixture
4mol ratio 1.3:3 sends into rotary kiln 10 and calcines, and at 1100 ℃, reacts 4h, obtains containing the tail gas that sulfurous gas volume fraction is 25% and the solid slag that is 75% containing calcium oxide massfraction.The tail gas clean-up of tornado dust collector 4 is except sending to sulfuric acid apparatus sulfuric acid processed with together with the tail gas of one-level cyclone preheater 7 after sulfur vapor.
Raw material 1: citric acid gypsum powder.Table 9 is its chemical composition.
Raw material 2: sulphur (purity 99.8wt%)
Table 9 citric acid gypsum powder chemical composition
Fuel: coking coal.Table 10 is its chemical composition.
Table 10 bituminous coal chemical composition
| Component | Fixed carbon | Volatile matter | Ash content | Moisture |
| Content/wt% | 56.0 | 20.6 | 17.8 | 5.6 |
Solid sulfur is in the interior Molten sulphur that obtains 140 ℃ through saturated vapor indirect heat exchange of sulfur melting groove 11; Molten sulphur feeds molten sulfur vapourizing furnace 9 through liquid sulfur pump 12 sulfur melting groove 11 is interior, and the waste heat tail gas of discharging with rotary kiln 10 kiln tails carries out indirect heat exchange, and making Molten sulphur gasification is the sulfur vapor of the 500 ℃ wind furnace 2 that reduces phlegm and internal heat, and waste heat tail gas enters secondary cyclone preheater 8; The interior mean particle size of feed bin 5 be 30 μ m gypsum raw meal powder by with mixed flue gas mark condition volume ratio be that 1:10000 feeds one-level cyclone preheater 7 through feeding machine 6, be warming up to 350 ℃, raw material through one-level preheating enter secondary cyclone preheater 8, be warming up to 600 ℃, enter together with the solid materials that spouted fluidized bed 3, a part discharge with spouted fluidized bed and enter rotary kiln through a raw material part for secondary preheating; Fuel forms hot flue gas with the air that gas blower 1 blasts by air excess 10% mixed firing in hotblast stove 2, the gas sulphur of molten sulfur vapourizing furnace 9 and hot flue gas by volume 1:0.2 are mixed, consume the superfluous oxygen in hot flue gas, form the mixed flue gas of 600 ℃, mixed air enters spouted fluidized bed 3; Preheated raw meal is carried out spouted fluidized heat exchange decomposition reaction with the mixed flue gas of gassiness sulphur at 600 ℃ in spouted fluidized bed 3; Tail gas enters tornado dust collector 4, and the powder under tornado dust collector 4 separate returns to spouted fluidized bed 3, and the solid materials after decomposition reaction is discharged through overflow port; Solid materials mixes with the gypsum raw meal powder of process secondary preheating, controls CaS and CaSO in mixture
4mol ratio 1.5:3 sends into rotary kiln 10 and calcines, and at 1300 ℃, reacts 0.5h, obtains containing the tail gas that sulfurous gas volume fraction is 8% and the solid slag that is 24% containing calcium oxide massfraction.The tail gas clean-up of tornado dust collector 4 is except sending to sulfuric acid apparatus sulfuric acid processed with together with the tail gas of one-level cyclone preheater 7 after sulfur vapor.
Embodiment 6
Raw material 1: nickel terra alba.Table 11 is its chemical composition.
Raw material 2: sulphur (purity 99.8wt%)
Table 11 nickel terra alba chemical composition
Fuel: Sweet natural gas.Table 12 is its chemical composition.
Table 12 natural gas chemistry composition
| Component | CH 4 | C 2H 6 | C 3H 8 | CO 2 | N 2 |
| Content/vol% | 97.23 | 0.18 | 0.07 | 1.3 | 1.22 |
Solid sulfur is in the interior Molten sulphur that obtains 145 ℃ through saturated vapor indirect heat exchange of sulfur melting groove 11; Molten sulphur feeds molten sulfur vapourizing furnace 9 through liquid sulfur pump 12 sulfur melting groove 11 is interior, and the waste heat tail gas of discharging with rotary kiln 10 kiln tails carries out indirect heat exchange, and making Molten sulphur gasification is the sulfur vapor of the 650 ℃ wind furnace 2 that reduces phlegm and internal heat, and waste heat tail gas enters secondary cyclone preheater 8; The interior mean particle size of feed bin 5 be 80 μ m gypsum raw meal powder by with mixed flue gas mark condition volume ratio be that 1:6000 feeds one-level cyclone preheater 7 through feeding machine 6, be warming up to 150 ℃, raw material through one-level preheating enter secondary cyclone preheater 8, be warming up to 350 ℃, enter together with the solid materials that spouted fluidized bed 3, a part discharge with spouted fluidized bed and enter rotary kiln through a raw material part for secondary preheating; Fuel forms hot flue gas with the air that gas blower 1 blasts by air excess 15% mixed firing in hotblast stove 2, the gas sulphur of molten sulfur vapourizing furnace 9 and hot flue gas by volume 1:3 are mixed, consume the superfluous oxygen in hot flue gas, form the mixed flue gas of 700 ℃, mixed air enters spouted fluidized bed 3; Preheated raw meal is carried out spouted fluidized heat exchange decomposition reaction with the mixed flue gas of gassiness sulphur at 550 ℃ in spouted fluidized bed 3; Tail gas enters tornado dust collector 4, and the powder under tornado dust collector 4 separate returns to spouted fluidized bed 3, and the solid materials after decomposition reaction is discharged through overflow port; Solid materials mixes with the gypsum raw meal powder of process secondary preheating, controls CaS and CaSO in mixture
4mol ratio 1.0:3 sends into rotary kiln 10 and calcines, and at 900 ℃, reacts 4h, obtains containing the tail gas that sulfurous gas volume fraction is 12% and the solid slag that is 48% containing calcium oxide massfraction.The tail gas clean-up of tornado dust collector 4 is except sending to sulfuric acid apparatus sulfuric acid processed with together with the tail gas of one-level cyclone preheater 7 after sulfur vapor.
Embodiment 7
Raw material 1: titanium dioxide by-product gypsum powder.Table 13 is its chemical composition.
Raw material 2: sulphur (purity 99.8wt%)
Table 13 titanium dioxide by-product gypsum powder chemical composition
Fuel: high sulphur coal.Table 14 is its technical analysis.
The technical analysis of table 14 high sulphur coal
| Component | Fixed carbon | Volatile matter | Ash content | Moisture |
| Content/wt% | 57.8 | 24.6 | 13.8 | 3.8 |
Solid sulfur is in the interior Molten sulphur that obtains 120 ℃ through saturated vapor indirect heat exchange of sulfur melting groove 11; Molten sulphur feeds molten sulfur vapourizing furnace 9 through liquid sulfur pump 12 sulfur melting groove 11 is interior, and the waste heat tail gas of discharging with rotary kiln 10 kiln tails carries out indirect heat exchange, and making Molten sulphur gasification is the sulfur vapor of the 450 ℃ wind furnace 2 that reduces phlegm and internal heat, and waste heat tail gas enters secondary cyclone preheater 8; The interior mean particle size of feed bin 5 be 40 μ m gypsum raw meal powder by with mixed flue gas mark condition volume ratio be that 1:7000 feeds one-level cyclone preheater 7 through feeding machine 6, be warming up to 100 ℃, raw material through one-level preheating enter secondary cyclone preheater 8, be warming up to 300 ℃, enter together with the solid materials that spouted fluidized bed 3, a part discharge with spouted fluidized bed and enter rotary kiln through a raw material part for secondary preheating; Fuel forms hot flue gas with 30% oxygen-rich air that gas blower 1 blasts by air excess 5% mixed firing in hotblast stove 2, the gas sulphur of molten sulfur vapourizing furnace 9 and hot flue gas by volume 1:5 are mixed, consume the superfluous oxygen in hot flue gas, form the mixed flue gas of 800 ℃, mixed air enters spouted fluidized bed 3; Preheated raw meal is carried out spouted fluidized heat exchange decomposition reaction with the mixed flue gas of gassiness sulphur at 600 ℃ in spouted fluidized bed 3; Tail gas enters tornado dust collector 4, and the powder under tornado dust collector 4 separate returns to spouted fluidized bed 3, and the solid materials after decomposition reaction is discharged through overflow port; Solid materials mixes with the gypsum raw meal powder of process secondary preheating, controls CaS and CaSO in mixture
4mol ratio 1.2:3 sends into rotary kiln 10 and calcines, and at 1100 ℃, reacts 3h, obtains containing the tail gas that sulfurous gas volume fraction is 20% and the solid slag that is 67% containing calcium oxide massfraction.The tail gas clean-up of tornado dust collector 4 is except sending to sulfuric acid apparatus sulfuric acid processed with together with the tail gas of one-level cyclone preheater 7 after sulfur vapor.
Raw material 1: natural gesso.Table 15 is its chemical composition.
Raw material 2: sulphur (purity 99.8wt%)
Table 15 natural gesso chemical composition
Fuel: hard coal.Table 16 is its technical analysis.
The technical analysis of table 16 hard coal
| Component | Fixed carbon | Volatile matter | Ash content | Moisture |
| Content/wt% | 70.0 | 4.3 | 20.5 | 5.2 |
Solid sulfur is in the interior Molten sulphur that obtains 150 ℃ through saturated vapor indirect heat exchange of sulfur melting groove 11; Molten sulphur feeds molten sulfur vapourizing furnace 9 through liquid sulfur pump 12 sulfur melting groove 11 is interior, and the waste heat tail gas of discharging with rotary kiln 10 kiln tails carries out indirect heat exchange, and making Molten sulphur gasification is the sulfur vapor of the 550 ℃ wind furnace 2 that reduces phlegm and internal heat, and waste heat tail gas enters secondary cyclone preheater 8; The interior mean particle size of feed bin 5 be 180 μ m gypsum raw meal powder by with mixed flue gas mark condition volume ratio be that 1:8000 feeds one-level cyclone preheater 7 through feeding machine 6, be warming up to 300 ℃, raw material through one-level preheating enter secondary cyclone preheater 8, be warming up to 550 ℃, enter together with the solid materials that spouted fluidized bed 3, a part discharge with spouted fluidized bed and enter rotary kiln through a raw material part for secondary preheating; Fuel forms hot flue gas with the air that gas blower 1 blasts by air excess 12% mixed firing in hotblast stove 2, the gas sulphur of molten sulfur vapourizing furnace 9 and hot flue gas by volume 1:0.5 are mixed, consume the superfluous oxygen in hot flue gas, form the mixed flue gas of 600 ℃, mixed air enters spouted fluidized bed 3; Preheated raw meal is carried out spouted fluidized heat exchange decomposition reaction with the mixed flue gas of gassiness sulphur at 550 ℃ in spouted fluidized bed 3; Tail gas enters tornado dust collector 4, and the powder under tornado dust collector 4 separate returns to spouted fluidized bed 3, and the solid materials after decomposition reaction is discharged through overflow port; Solid materials mixes with the gypsum raw meal powder of process secondary preheating, controls CaS and CaSO in mixture
4mol ratio 1.1:3 sends into rotary kiln 10 and calcines, and at 1000 ℃, reacts 5h, obtains containing the tail gas that sulfurous gas volume fraction is 13% and the solid slag that is 60% containing calcium oxide massfraction.The tail gas clean-up of tornado dust collector 4 is except sending to sulfuric acid apparatus sulfuric acid processed with together with the tail gas of one-level cyclone preheater 7 after sulfur vapor.
Raw material 1: natural anhydrite powder.Table 17 is its chemical composition.
Raw material 2: sulphur (purity 99.8wt%)
Table 17 anhydrite powder chemical composition
Fuel: Sweet natural gas.Table 18 is its chemical composition.
Table 18 natural gas chemistry composition
| Component | CH 4 | C 2H 6 | C 3H 8 | CO 2 | N 2 |
| Content/vol% | 97.23 | 0.18 | 0.07 | 1.3 | 1.22 |
Solid sulfur is in the interior Molten sulphur that obtains 135 ℃ through saturated vapor indirect heat exchange of sulfur melting groove 11; Molten sulphur feeds molten sulfur vapourizing furnace 9 through liquid sulfur pump 12 sulfur melting groove 11 is interior, and the waste heat tail gas of discharging with rotary kiln 10 kiln tails carries out indirect heat exchange, and making Molten sulphur gasification is the sulfur vapor of the 650 ℃ wind furnace 2 that reduces phlegm and internal heat, and waste heat tail gas enters secondary cyclone preheater 8; The interior mean particle size of feed bin 5 be 40 μ m gypsum raw meal powder by with mixed flue gas mark condition volume ratio be that 1:4500 feeds one-level cyclone preheater 7 through feeding machine 6, be warming up to 250 ℃, raw material through one-level preheating enter secondary cyclone preheater 8, be warming up to 500 ℃, enter together with the solid materials that spouted fluidized bed 3, a part discharge with spouted fluidized bed and enter rotary kiln through a raw material part for secondary preheating; Fuel forms hot flue gas with the air that gas blower 1 blasts by air excess 10% mixed firing in hotblast stove 2, the gas sulphur of molten sulfur vapourizing furnace 9 and hot flue gas by volume 1:8 are mixed, consume the superfluous oxygen in hot flue gas, form the mixed flue gas of 750 ℃, mixed air enters spouted fluidized bed 3; Preheated raw meal is carried out spouted fluidized heat exchange decomposition reaction with the mixed flue gas of gassiness sulphur at 650 ℃ in spouted fluidized bed 3; Tail gas enters tornado dust collector 4, and the powder under tornado dust collector 4 separate returns to spouted fluidized bed 3, and the solid materials after decomposition reaction is discharged through overflow port; Solid materials mixes with the gypsum raw meal powder of process secondary preheating, controls CaS and CaSO in mixture
4mol ratio 1.3:3 sends into rotary kiln 10 and calcines, and at 1300 ℃, reacts 1h, obtains containing the tail gas that sulfurous gas volume fraction is 15% and the solid slag that is 55% containing calcium oxide massfraction.The tail gas clean-up of tornado dust collector 4 is except sending to sulfuric acid apparatus sulfuric acid processed with together with the tail gas of one-level cyclone preheater 7 after sulfur vapor.
Comparative example
The method decomposing phosphogypsum that adopts CN101708826A to announce; it first carries out preheating phosphogypsum in preheating decomposing phosphogypsum process under protection of inert gas; pass into again sulfur vapor and carry out reduction reaction; this process is intermittent operation, trivial operations; and the preheating phosphogypsum stage can be wasted a large amount of rare gas elementes; entirety decomposing phosphogypsum process need a large amount of human assistance, simultaneously also inconvenient for the collection of solid slag of preparing sulfurated lime workshop section output, cannot realize industrial automation and produce.
And this patent adopts spouted bed can greatly increase the contact area of phosphogypsum and sulphur steam as the reactor of preparing sulfurated lime workshop section, improve reaction efficiency, utilized in CN101708826A patent sulfurated lime and the needed non-oxidizable high-temperature gas of phosphogypsum roasting for the phosphogypsum of pre-hot preparation sulfurated lime simultaneously, can significant energy efficient, greatly save in CN101708826A patent rare gas element usage quantity required in phosphogypsum warm.In this patent, to prepare the protection gas of sulfurated lime process be hot flue gas to decomposing ardealite; its with sulphur vapor mixing to a certain extent after together with as reaction atmosphere time also for reaction provides required heat and decomposition temperature; the reaction that makes like this phosphogypsum prepare sulfurated lime process is simplified more; the collection of simultaneously preparing sulfurated lime workshop section solid slag is also more convenient, and this produces greatly favourable for realizing industrial automation.
Claims (10)
1. the spouted fluidized decomposition technique of gypsum, is characterized in that, comprises the following steps:
(1), sulphur is heated to 120 ℃～150 ℃ in sulfur melting groove, obtain Molten sulphur;
(2), Molten sulphur is through liquid sulfur pump feeding molten sulfur vapourizing furnace, the waste heat tail gas of discharging with rotary kiln tail carries out heat exchange, makes Molten sulphur gasification be warming up to 450 ℃～750 ℃, the waste heat tail gas after heat exchange enters secondary cyclone preheater;
(3), in feed bin mean particle size be 1 μ m～200 μ m gypsum raw meal powder in the waste heat tail gas mark condition volume ratio ratio that is 1:4000～10000, carry out heat exchange through feeding machine feeding one-level cyclone preheater and waste heat tail gas, be warming up to 50 ℃～400 ℃, raw material after the preheating of one-level cyclone preheater enter secondary cyclone preheater and waste heat tail gas carries out heat exchange, be warming up to 200 ℃～700 ℃, enter together with the solid materials that spouted fluidized bed, a part discharge with spouted fluidized bed and enter rotary kiln through a raw material part for secondary cyclone preheater preheating; The waste heat tail gas of discharging after the heat exchange of secondary cyclone preheater enters the heat exchange of one-level cyclone preheater;
(4) fully burning after the air mixed that, fuel blasts with gas blower in hotblast stove, the sulfur gas that the hot flue gas producing and molten sulfur vapourizing furnace come by volume 0.2～10:1 is mixed, consume the remaining oxygen in hot flue gas, form the mixed flue gas containing sulfur vapor of 600 ℃～1100 ℃, mixed flue gas enters spouted fluidized bed;
(5), in spouted fluidized bed, carry out spouted fluidized heat exchange decomposition reaction with the mixed flue gas containing sulfur vapor through the raw material of secondary preheating at 500 ℃～1000 ℃, the solid materials after decomposition reaction is discharged through overflow port; Fluidized-bed tail gas enters tornado dust collector, and the powder under separating returns to spouted fluidized bed;
(6), the solid materials of the step 5 gained pre-plaster of paris raw meal powder with step 3 mixes, and controls CaS and CaSO in mixture
4mol ratio is that 1.0～1.5:3 sends into rotary kiln, at 800 ℃～1300 ℃, reacts 0.5～5 hour, obtains containing the tail gas of sulfurous gas and the solid slag containing calcium oxide.
2. gypsum spouted fluidized bed decomposition technique according to claim 1, is characterized in that, the tail gas that in step (5), spouted fluidized bed is discharged purifies through tornado dust collector, and isolated powder returns to spouted liquefied bed.
3. gypsum spouted fluidized bed decomposition technique according to claim 2, is characterized in that, through cyclone dust removal tail gas after treatment, then after sulphur removal vapour cure, is transported in the device of preparing sulfuric acid, for the preparation of sulfuric acid.
4. gypsum spouted fluidized bed decomposition technique according to claim 1, is characterized in that, the tail gas that the one-level cyclone preheater in step (3) is discharged is transported in the device of preparing sulfuric acid, for the preparation of sulfuric acid.
5. gypsum spouted fluidized bed decomposition technique according to claim 1, is characterized in that, the air that described fuel blasts with gas blower in hotblast stove is fully burning after mixing by air excess 5%～15%.
6. gypsum spouted fluidized bed decomposition technique according to claim 1 or 5, is characterized in that, the oxygen-rich air burning that described fuel blasts oxygen level 25-50% through gas blower in hotblast stove produces hot flue gas.
7. gypsum spouted fluidized bed decomposition technique according to claim 1, is characterized in that, described fuel is at least one in Sweet natural gas, coal gas, liquefied petroleum gas (LPG), hard coal, bituminous coal or high sulphur coal.
8. gypsum spouted fluidized bed decomposition technique according to claim 7, is characterized in that, described fuel is high sulphur coal.
9. gypsum spouted fluidized bed decomposition technique according to claim 1, it is characterized in that, described gypsum is at least one in phosphogypsum, desulfurated plaster, salt gypsum, fluorgypsum, citric acid gypsum, nickel gypsum, titanium dioxide by-product gypsum, the plaster of paris, anhydrite.
10. gypsum spouted fluidized bed decomposition technique according to claim 1, is characterized in that, gypsum spouted fluidized bed decomposition technique as above, and gypsum raw meal powder is continuous dosing, the spouted fluidized decomposing and calcining system of gypsum raw meal powder is continuous flow procedure.
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| CN104555946A (en) * | 2015-01-20 | 2015-04-29 | 上海三夫工程技术有限公司 | Method for jointly producing sulphuric acid and cement clinker by using sulphur gas to reduce gypsum |
| CN105858620A (en) * | 2016-05-20 | 2016-08-17 | 四川大学 | Method for decomposing gypsum through synergistic fluidization |
| CN109809456A (en) * | 2019-03-13 | 2019-05-28 | 山东大学 | A kind of system and method for coal gasification collaboration gypsum calcining coproduction calcium oxide and sulphur |
| CN113148961A (en) * | 2021-03-31 | 2021-07-23 | 云南云天化环保科技有限公司 | System and process for preparing high-concentration sulfur dioxide flue gas by using phosphogypsum |
| CN113912021A (en) * | 2021-11-16 | 2022-01-11 | 上海驰春节能科技有限公司 | System and process for producing sulfur and cement clinker by using industrial byproduct gypsum and metallurgical slag melt |
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| CN201737711U (en) * | 2010-03-24 | 2011-02-09 | 江苏省一夫新材料科技有限公司 | Chemical gypsum decomposing device |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104555946A (en) * | 2015-01-20 | 2015-04-29 | 上海三夫工程技术有限公司 | Method for jointly producing sulphuric acid and cement clinker by using sulphur gas to reduce gypsum |
| CN105858620A (en) * | 2016-05-20 | 2016-08-17 | 四川大学 | Method for decomposing gypsum through synergistic fluidization |
| CN109809456A (en) * | 2019-03-13 | 2019-05-28 | 山东大学 | A kind of system and method for coal gasification collaboration gypsum calcining coproduction calcium oxide and sulphur |
| CN109809456B (en) * | 2019-03-13 | 2021-02-26 | 山东大学 | System and method for co-producing calcium oxide and sulfur by coal gasification and gypsum calcination |
| CN113148961A (en) * | 2021-03-31 | 2021-07-23 | 云南云天化环保科技有限公司 | System and process for preparing high-concentration sulfur dioxide flue gas by using phosphogypsum |
| CN113148961B (en) * | 2021-03-31 | 2023-05-30 | 云南云天化环保科技有限公司 | System and process for preparing high-concentration sulfur dioxide flue gas by using phosphogypsum |
| CN113912021A (en) * | 2021-11-16 | 2022-01-11 | 上海驰春节能科技有限公司 | System and process for producing sulfur and cement clinker by using industrial byproduct gypsum and metallurgical slag melt |
| CN113912021B (en) * | 2021-11-16 | 2022-12-20 | 上海驰春节能科技有限公司 | System and process for producing sulfur and cement clinker by using industrial byproduct gypsum in cooperation with metallurgical slag solution |
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