CN101559930B - Discarded gypsum kinetic wave sulfuric acid production process method and execution device thereof - Google Patents
Discarded gypsum kinetic wave sulfuric acid production process method and execution device thereof Download PDFInfo
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- CN101559930B CN101559930B CN2009100592889A CN200910059288A CN101559930B CN 101559930 B CN101559930 B CN 101559930B CN 2009100592889 A CN2009100592889 A CN 2009100592889A CN 200910059288 A CN200910059288 A CN 200910059288A CN 101559930 B CN101559930 B CN 101559930B
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Abstract
The invention discloses a discarded gypsum kinetic wave sulfuric acid production process method and an execution device thereof. The method comprises the following steps: adding discarded gypsum, smokeless solid fuel powder and primary air into a kinetic wave reactor; suspending the raw materials in a reduction combustion area for carrying out a reduction reaction; introducing secondary air into an oxidation combustion area so as to further oxidize and combust the residual raw materials from the reduction combustion reaction; discharging reaction gas after the combustion reaction through the kinetic wave reactor; after the purification by a purifying device, passing the reaction product into a converter for a conversion reaction; and after the conversion reaction, passing the reaction product into an absorption column for absorption and then obtaining sulfuric acid. The weight content of the solid fuel is the demand quantity meeting the requirement that the raw material gypsum is fullyreduced, oxidized and converted. When the discarded gypsum is used to produce the sulfuric acid via the method, the dissociation rate of calcium sulfate reaches 98 percent, the concentration of SO2 in the gas reaches 6 to 15 percent, and the discharged solid refuse can be used as semi-clinker for cement production or other products. The industrialization of the sulfuric acid creates immeasurablevalue for the comprehensive use of the discarded gypsum.
Description
Technical field
The present invention relates to discarded gypsum treatment technology, particularly relate to discarded gypsum resource comprehensive reutilization, more specifically, is about being raw material production vitriolic processing method with discarded gypsum.
Background technology
In China, about 2,500 ten thousand tons of phosphorous chemical industry enterprise year discharging phosphogypsum, about 2,500 ten thousand tons of thermal power plant's year discharging desulfurated plaster, about 3,000,000 tons of the waste gypsum of the annual discharging of industries such as fluorine chemical and citric acid production, national industrial waste gypsum total amount can reach 53,000,000 tons.The phosphogypsum quantity of annual discharging is huge, serious environment pollution not only, and occupy a large amount of soils.This situation has begun the development of industry of severe inhibition phosphorus ammonium and relevant industries, and the outlet that therefore solves the industrial waste gypsum has become the very urgent problem demanding prompt solution of scientific and technical personnel.
The industrial waste gypsum is pressed oxide compound metering, and it is about 30% generally to contain CaO, SO
3About 36%, also contain essences such as silicon, iron, aluminium, magnesium in addition.The resource utilization of waste gypsum and utilize many approach are arranged wherein utilizes the industrial waste gypsum to produce sulfuric acid, returns the original production flow process again as raw material, is the approach of a recycling economy to phosphorous chemical industry enterprise.Produce the vitriolic method in China with the industrial waste gypsum at present and have only the rotary kiln method, promptly add fuel and the common roasting of gypsum in the rotary kiln ingress, the sulfur dioxide gas that discharges is produced sulfuric acid through transforming to absorb, residuum is cement clinkers such as Calucium Silicate powder, promptly finishes the process that gypsum is resolved into sulfurous gas and cement baking in same kiln body.
Research is recycled in the chemical industry of industrial waste gypsum resource, starts from nineteen eighty-three, has finished the test of 7000t/a salt gypsum system producing sulfuric acid and jointly Cement industry jointly by Wudi County, Shandong vitriol works, abundant Xinghua, Jinan factory, Shandong Chemical Inst.1984, YUNLAN Phosphor Fertilizer Plant was carried out the commerical test of by-product phosphogypsum system sulfuric acid and cement.The nineties, for the phosphogypsum that produces to ammonium phosphate plant finds new outlets, former the Ministry of Chemical Industry at Lubei Chemical Plant's investment construction one cover scale with produce the supporting phosphogypsum system 40,000 t/a sulfuric acid of 30,000 t phosphorus ammoniums per year, the demonstration unit (being called for short 346 engineerings) of the 60000 t/a cement of coproduction simultaneously, to improve previous type approval test work, the accumulation knowhow.The mid-90, the phosphatization factory on ground such as former State Planning Commission, former the Ministry of Chemical Industry ratify in the Shifang, Yin Shan, western Shandong, Shenyang, Laixi, Zunhua has set up many covers phosphorus ammonium-sulfuric acid-cement joint production device.But these devices, because have that energy consumption is big in raw material phosphogypsum composition instability, the production process, production cost is high, cement quality is unstable in the production process, many technical problems to be solved such as sulfur-bearing is low in the gas, at present can utilize salt gypsum that self sea salt chemical industry obtains except Lubei Chemical Plant and adjusted production process continued to move by torch firing sulphur, the system of other six tame phosphogypsum co-producing sulfuric acid and cement closes down in succession.
There is the Phalaborwa Bosveld Kunsmis factory in OSW-Krupp, M ü lller-K ü hne, Linz company and South Africa in the enterprise of overseas utilization phosphogypsum production sulfuric acid and cement at present, their technical process is similar, all be to adopt the phosphogypsum behind the calcined dehydration is sent into rotary kiln decomposition system gas, gained gas is behind clean units such as electric precipitator, washer, moisture eliminator, obtain sulphur trioxide by convertor, obtain sulfuric acid through absorption.The solid slag that ejects from rotary kiln obtains cement through adding the grinding of auxiliary material and grinding machine.Linz chemical company improved phosphogypsum sulfuric acid-cement plant in 1972, had set up the counterflow heat exchanger of Krupp company at the feed end of rotary kiln, and Phalaborwa factory has also adopted this heat exchanger.In this heat exchanger, can make the energy consumption of rotary kiln reduce 15%～20% behind charging and the rotary kiln tail gas countercurrent flow.
Linz company and Phalaborwa factory all adopt single rotary kiln.The long 70.7m of the rotary kiln of Linz has expanding reach.The diameter at two ends is 2.8m, and the diameter of expanding reach is 3.0m.Throughput when the Krupp heat exchanger is not set is about 200t cement clinker/d, and the throughput that is provided with behind the heat exchanger is about 230t/d.The rotary kiln diameter 3.8m of Phalaborwa factory, long 107m, throughput is daily output cement clinker 320～350t.The rotary kiln of prior art is combined with the Krupp heat exchanger, can design the separate unit rotary kiln of daily output 600t grog, this production-scale rotary kiln, its internal diameter are 5.5m, long 120m.Expection can design the rotary kiln of daily output 1000t grog in the future.Claim that according to Linz company the minimum economic size of factory is 500t/d, promptly produce 150000 tons of cement clinkers per year.The plant investment of this scale is 5 times of equal scale plant investment of burning sulphur.
Rotary kiln technology is actually and finishes gypsum decomposition system gas and cement sintering process in same kiln body.Because gypsum decomposes and the required condition of cement sintering and inequality, so exist energy consumption higher in this flow process, sulfur dioxide concentration is low in the gas, factors such as cement quality instability, and heat transfer and mass-transfer efficiency are low simultaneously.At rotary kiln conduct heat and mass transfer aspect inefficiency, the research of external decomposition outside just having carried out other type of decomposition reactor and kiln not long ago.People such as U.S. Wheelock have just finished the test of two-stage fluidized decomposing phosphogypsum in nineteen ninety.Germany Lurgi company has carried out the research work with the fluidised bed decomposition phosphogypsum.The outer decomposition of kiln can be satisfied gypsum better and decompose required condition, makes it more energy-conservation.The development trend of cement industry itself also is to decompose development outside kiln at present.But decomposition system solid/liquid/gas reactions and heat transfer efficiency that prior art utilizes gypsum to produce in the sulfuric acid process are high not enough, can't be satisfactory.
Summary of the invention:
The present invention is directed to the discarded gypsum of prior art utilization and produce the deficiency that sulfuric acid exists, disclose a kind of new gypsum that utilizes and produce the vitriolic processing method---discarded gypsum kinetic wave sulfuric acid production process method, and the equipment that is used for its enforcement, produce that sulfuric acid exists because the low calcium sulfate rate of decomposition that causes of mass-transfer efficiency is low to solve the discarded gypsum of prior art utilization, the concentration of sulfurous gas is low in the gas, and because the low problems such as energy consumption height that cause of heat transfer efficiency, abundant discarded gypsum is produced the vitriolic technology.
Above-mentioned technical problem to be solved by this invention can realize by the discarded gypsum kinetic wave sulfuric acid production process method that is made of following technical scheme.
Discarded gypsum kinetic wave sulfuric acid production process method disclosed by the invention is: will contain discarded gypsum of dehydration and smokeless solid-fuelled mixed powder raw material and a wind air and join the dynamic wave reactor, make it to be suspended in the reduction combustion zone that the power corrugated that formed by the reduction burning is separated into and carry out reduction reaction, the oxidizing fire district that is separated on the power corrugated feeds the secondary air air, make the raw material of reduction combustion reactions remnants be able to further oxidizing fire, reactant gases after the combustion reactions is discharged by the dynamic wave reactor, send into and after treating plant purifies, enter convertor and carry out conversion reaction, send into the absorption tower after the conversion reaction again and promptly make sulfuric acid through absorbing, in described mixed powder raw material, smokeless solid-fuelled weight content makes discarded gypsum obtain the amount that abundant reduction-oxidation transforms needs for satisfying.
In above-mentioned discarded gypsum kinetic wave sulfuric acid production process, the temperature in the dynamic wave reactor should not be lower than smokeless solid-fuelled burning-point; After preferably being preheated to 200-400 ℃, described mixed powder raw material joins the dynamic wave reactor again; The secondary air air that joins the oxidizing fire district preferentially adopts the warm air of temperature 200-400 ℃ of scope.
In above-mentioned discarded gypsum kinetic wave sulfuric acid production process method, can be used to produce cement in order to make the solid slag of discharging from the dynamic wave reactor, also can contain silicon compound in the described mixed powder raw material or/and iron cpd.Silicon compound in the mixed powder raw material is or/and the content of iron cpd, can determine its content according to the manufacture of cement aequum of filling a prescription.
Above-mentioned discarded gypsum kinetic wave sulfuric acid production process method, can regulate by composition of raw materials according to the purposes needs from the solid slag that the dynamic wave reactor is discharged, can obtain materials such as calcium oxide, Calucium Silicate powder uses it for anything else, for example, can deliver to rotary kiln and produce cement, also can be used as the output of product calcium oxide, offer the industry that needs calcium oxide, as material of construction, smelting industry, calcium carbide production industry etc.In the time will consolidating slag and be used to produce cement, normally the solid slag of discharging with produce the required batching of cement and directly join cement kiln and carry out manufacture of cement from the dynamic wave reactor.In order to reduce the energy consumption in the discarded gypsum kinetic wave sulfuric acid production process, preferably use from the cement kiln expellant gas raw material of sending into the dynamic wave reactor is carried out preheating.
Be used to implement the equipment of the above discarded gypsum kinetic wave sulfuric acid production process method, described dynamic wave reactor can be designed to the power corrugated and be planar dynamic wave reactor, this dynamic wave reactor, its bottom design has some as a wind air intlet that forms fluidized-bed layer, design has material inlet on the reactor cylinder body wall, Gu slag outlet and some secondary air air intlets, wherein material inlet and solid slag outlet are positioned at the reduction combustion zone, the secondary air air intlet is positioned at the oxidizing fire district, the reactor top design gas discharge outlet that responds, design has and purges bed and prevent the jet air import that scabs near the barrel wall at the bottom of the reactor cylinder.
Also the dynamic wave reactor design can be become the power corrugated to be the dynamic wave reactor of ellipsoid, this dynamic wave reactor, its tip designs has makes raw material and wind air mixed enter inlet device in the reactor in the effusive mode, the design of reactor bottom has solid slag outlet, design the pneumatic outlet that responds on the reactor cylinder body wall, some secondary air air intlets and heating are burnt and are chewed, reaction gas outlet is positioned at reactor cylinder body wall top, secondary air air intlet and heating are burnt to chew and are arranged on reactor cylinder body wall middle part and make the secondary air air can surround the reduction combustion zone, and design has and purges the tube end and prevent the jet air import that scabs near the barrel wall at the bottom of the reactor cylinder.
As the dynamic wave reactor of the specific equipment that is used to implement discarded gypsum kinetic wave sulfuric acid production process method, its power corrugated also can be designed to multiple corrugateds such as column face, irregular except the corrugated, plane that can be designed to the above, ellipsoid corrugated.
Discarded gypsum kinetic wave sulfuric acid production process method provided by the invention, its core are to have adopted combustion powered ripple reactor.The dynamic wave reactor has two important feature, and the corrugated that the first utilizes the fluid combustion dynamic process to produce will reduce the space to isolate relatively, be reflected under the weakly reducing atmosphere with assurance and carry out.Oxidation side on combustion powered corrugated feeds secondary air, and the inflammable gas of remnants is burnt, and simultaneously with residual phosphorus oxidation, the heat of gained imports the reduction space into to reclaim heat energy through radiation.Be provided with jet in the bed on the other hand, can in time purge bed, scab preventing.In different humidity provinces different reactions takes place in the dynamic wave reactor, the principal reaction process is as follows.
The reaction that takes place under 900～1100 ℃ of temperature is:
CaSO
4+2C→CaS+2CO
2↑ΔH
0＝525.0kJ/mol
The reaction that takes place under 1150～1200 ℃ of temperature is:
CaSO
4+(1/3)CaS→(4/3)CaO+(4/3)SO
2↑ΔH
0＝1269.1kJ/mol
The total reaction that takes place in the dynamic wave reactor is:
CaSO
4+(1/2)C→CaO+SO
2↑+(1/2)CO
2↑
Temperature of reaction in the dynamic wave reactor can reduce by adding suitable additive, as adding silicon compound, iron cpd etc.The Calucium Silicate powder that the silicon compound that adds generates can be used as the usefulness of producing cement clinker.
The present invention adopts combustion powered ripple novel reactor that gypsum is carried out kiln to decompose outward, because the distinctive working mechanism of dynamic wave reactor, the decomposition mass-transfer efficiency of gypsum in the dynamic wave reactor is very high, and the calcium sulfate rate of decomposition in the gypsum can reach 98%, SO from the reactor expellant gas
2Concentration can be up to 6%～10%.Salvage stores after the desulfurization can be delivered to the sintering oven calcination of cement clinker and make the usefulness of other products.The combustion powered ripple oxidizing atmosphere that forms in the dynamic wave reactor bed can be quickened the decomposition of residual phosphorus, and the phosphorus content in the residue is reduced, and the quality of cement is improved.Adopt processing method of the present invention, can produce vitriolic production line next door at original pyrite concentrate and set up production system with less cost, gained gas is sent into original system in order to produce sulfuric acid.
The discarded gypsum kinetic wave sulfuric acid production process that the present invention proposes can be operated under stable gas concentration, Gu residual phosphorus amount is low in the slag, establishes for sulfuric acid and Cement Production and to have found solid foundation.The combustion powered ripple reactor that is adopted, because decomposition course mass transfer reaction and the heat transfer efficiency height of gypsum in the dynamic wave reactor, it is little therefore to have device body, and ability is big, and heat energy utilization fully waits advantage.Because the dynamic wave reactor is a static equipment, compare with rotary kiln in addition, hear rate is low by 30%, and power consumption is low by 40%, and upkeep cost also reduces greatly.Produce cement with the solid slag that the present invention discharges, grog sintering oven size is also much smaller than the rotary kiln of equal production capacity, invests also more low.The industrialization of this technology of the present invention will produce immeasurable value to comprehensive utilization of phosphogypsum.
Description of drawings
Accompanying drawing 1 is the technology schematic block diagram of an embodiment of processing method of the present invention.
Accompanying drawing 2 is technology schematic block diagrams of another embodiment of processing method of the present invention.
Accompanying drawing 3 is that the corrugated that processing method of the present invention adopts is a planar dynamic wave structure of reactor synoptic diagram.
Accompanying drawing 4 is that the corrugated that processing method of the present invention adopts is the dynamic wave structure of reactor synoptic diagram of ellipsoid.
In above-mentioned accompanying drawing, the sign object of each shown by reference numeral is as follows: 1 dynamic wave reactor; 2 dynamic wave corrugateds; 3 oxidizing fire districts; 4 reduction combustion zones.
Embodiment
To closing embodiment the present invention is specifically described below, so that personnel's the understanding of the present invention of affiliated technical field.Be necessary what this particularly pointed out to be; embodiment is used for just that the present invention will be further described; can not be interpreted as limiting the scope of the invention; affiliated art skilled person; to improvement and adjustment that the present invention makes non-intrinsically safe, still belong to protection scope of the present invention according to the foregoing invention content.
In following each embodiment, involved amounts of components per-cent or umber all are weight percentage or parts by weight except that specifying.
The present embodiment technical process as shown in Figure 1, the dynamic wave reactor that is adopted is corrugated, a plane dynamic wave reactor, its structure as shown in Figure 3.Blast a wind air about 300 ℃ by the dynamic wave reactor lower part, form fluidized-bed.The phosphogypsum that has dewatered (dihydrate gypsum CaO 30%, dehydration back 37%) 100 parts (all by weight), silica flour (SiO
290%) 6 parts (be controlled at 5～8 parts of scopes all can), 8 parts in hard coal (C 70%) (be controlled at 5.6～17.2 parts of scopes all can) be used the tail gas of discharging from rotary kiln to be preheated to about 250 ℃ at preheater to add from the dynamic wave reactor inlet.Temperature of reaction is controlled at 1280～1320 ℃ of scopes, 30～60 minutes residence time.The bed middle part blasts the secondary air air about 300 ℃, purges bed and prevents that the jet air that scabs from being added by the import near the reactor beds bottom.Contain SO 2 tail gas and drawn by the reactor top relief outlet, send into and enter convertor carry out conversion reaction after purification system purifies, the gas after the conversion reaction is sent into the absorption tower again and is promptly made sulfuric acid through absorbing.The solid slag of being discharged by the reactor-side below is that cement half product grog is sent into the manufacture of cement rotary kiln, add suitable batching loess, sal and ferriferous raw material by the silicate cement type of producing simultaneously, 1350～1450 ℃ of sintering temperatures 30 minutes, promptly obtain the cement products grog.
The present embodiment technical process as shown in Figure 2, the dynamic wave reactor that is adopted is an ellipsoid corrugated dynamic wave reactor, its structure as shown in Figure 4.Being positioned at the raw material of reactor top and the inlet device of a wind air is that the multi-flow burning is chewed, bring the sulphur gypsum of coal dust and dehydration into by about 300 ℃ that blast wind air, chew by burning and to enter reactor and form jet, the powder that sprays into and a wind-heat air become approximate elliposoidal under the compression of the secondary air air of about 300 ℃ of cyclic, and the heating burning are installed on the sustained height of secondary air chew.In high temp jet, add the sulphur gypsum (dehydration back 37%) 100 parts (all by weight) that has dewatered, 12 parts in hard coal (C70%) (be controlled at 8.4～20.1 parts of scopes all can), temperature of reaction is controlled at 1400～1600 ℃ of scopes, 10～30 seconds of the residence time.Drawn by the side of reactor top and to contain SO 2 tail gas, send into and enter convertor after purification system purifies and carry out conversion reaction, the gas after the conversion reaction is sent into the absorption tower again and is promptly made sulfuric acid through absorbing.The solid slag of being discharged below by reactor is calcium oxide half product.
Claims (10)
1. discarded gypsum kinetic wave sulfuric acid production process method, it is characterized in that, to contain discarded gypsum of dehydration and smokeless solid-fuelled mixed powder raw material and a wind air and join the dynamic wave reactor, make it to be suspended in the reduction combustion zone that the power corrugated that formed by the reduction burning is separated into and carry out reduction reaction, the oxidizing fire district that is separated on the power corrugated feeds the secondary air air, make the raw material of reduction combustion reactions remnants be able to further oxidizing fire, reactant gases after the combustion reactions is discharged by the dynamic wave reactor, send into and enter convertor after treating plant purifies and carry out conversion reaction, send into the absorption tower after the conversion reaction again and promptly make sulfuric acid through absorbing, in described mixed powder raw material, smokeless solid-fuelled weight content makes discarded gypsum obtain abundant reduction-oxidation conversion needs for satisfying.
2. discarded gypsum kinetic wave sulfuric acid production process method according to claim 1 is characterized in that the temperature in the dynamic wave reactor is not less than smokeless solid-fuelled burning-point.
3. discarded gypsum kinetic wave sulfuric acid production process method according to claim 1 is characterized in that described mixed powder raw material preheating joins the dynamic wave reactor again after 200-400 ℃.
4. discarded gypsum kinetic wave sulfuric acid production process method according to claim 1, the secondary air air that it is characterized in that joining the oxidizing fire district is that temperature is 200-400 ℃ a warm air.
5. discarded gypsum kinetic wave sulfuric acid production process method according to claim 1 is characterized in that also containing silicon compound or/and iron cpd in the described mixed powder raw material.
6. discarded gypsum kinetic wave sulfuric acid production process method according to claim 5 is characterized in that the silicon compound in the described mixed powder raw material or/and the content of iron cpd is the required definite content of production cement formula.
7. according to the described discarded gypsum kinetic wave sulfuric acid production process method of one of claim 1 to 6, it is characterized in that joining cement kiln from the solid slag that the dynamic wave reactor is discharged with the required batching of production cement produces cement.
8. discarded gypsum kinetic wave sulfuric acid production process method according to claim 7 is characterized in that using from the cement kiln expellant gas raw material is carried out preheating.
9. be used to implement the equipment of the described discarded gypsum kinetic wave sulfuric acid production process method of claim 1 to 8, it is characterized in that described dynamic wave reactor is planar dynamic wave reactor for the power corrugated, the reactor bottom design has some as a wind air intlet that forms fluidized-bed layer, design has material inlet on the reactor cylinder body wall, Gu slag outlet and some secondary air air intlets, wherein material inlet and solid slag outlet are positioned at the reduction combustion zone, the secondary air air intlet is positioned at the oxidizing fire district, the reactor top design gas discharge outlet that responds, design has and purges bed and prevent the jet air import that scabs near the barrel wall at the bottom of the reactor cylinder.
10. be used to implement the equipment of the described discarded gypsum kinetic wave sulfuric acid production process method of claim 1 to 8, it is characterized in that described dynamic wave reactor is the dynamic wave reactor of ellipsoid for the power corrugated, reactor top design has makes raw material and wind air mixed enter inlet device in the reactor with mode of jet, the design of reactor bottom has solid slag outlet, design the pneumatic outlet that responds on the reactor cylinder body wall, some secondary air air intlets and heating are burnt and are chewed, reaction gas outlet is positioned at reactor cylinder body wall top, secondary air air intlet and heating are burnt to chew and are arranged on reactor cylinder body wall middle part and make the secondary air air can surround the reduction combustion zone, and design has and purges the tube end and prevent the jet air import that scabs near the barrel wall at the bottom of the reactor cylinder.
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