CN104445212A - Method for processing fly ash used for circulating fluidized bed - Google Patents
Method for processing fly ash used for circulating fluidized bed Download PDFInfo
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- CN104445212A CN104445212A CN201310420532.6A CN201310420532A CN104445212A CN 104445212 A CN104445212 A CN 104445212A CN 201310420532 A CN201310420532 A CN 201310420532A CN 104445212 A CN104445212 A CN 104445212A
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Abstract
The invention relates to a method for processing fly ash used for a circulating fluidized bed, which comprises the following steps: dissolving fly ash from the circulating fluidized bed out by hydrochloric acid, filtering to obtain filter residue and a leaching liquid; adjusting pH value of the leaching liquid to 1.5-3.5 by ammoniacal liquor, deposing, filtering to obtain the filter residue and a filtrate, washing filter residue, drying to obtain a compound of iron; adjusting the pH value of the filtrate after extracting iron to 3.8-5.2 by the ammoniacal liquor, deposing, filtering to obtain the filter residue and the filtrate, washing filter residue, drying to obtain aluminium hydroxide, further calcining to obtain metallurgy alumina; adding magnesium oxide in an ammonium chloride solution after extracting aluminium and performing ammonia distilling and hydrolysis reactions to obtain hydrogen chloride gas, ammonia gas and magnesium oxide. According to the invention, stepwise extraction of useful elements such as aluminium, silicon and iron in fly ash can be realized, cycle utilization of the materials can be realized, process is simple, cost is low, and the method opens new approach for high value utilization of fly ash from the circulating fluidized bed.
Description
Technical field
The invention belongs to flyash higher value application field, particularly a kind of method utilizing step-by-step precipitation method to extract the useful elements such as aluminium, silicon and iron from circulating fluid bed coal ash.
Background technology
In recent years, bring the sharply increase of solid waste coal ash quantity discharged while the coal electricity industry of China develops rapidly, by 2007, the annual emissions of China's flyash more than 200,000,000 tons, and was still increasing year by year, and accumulative volume of cargo in storage is more than 2,500,000,000 tons.The flyash of a large amount of discharge had both taken a large amount of soil, and again to soil, water resources and air cause severe contamination.Therefore, the comprehensive utilization of flyash becomes the task of top priority.
At present, multiple fields such as flyash is building work, building are applied, although large usage quantity, its digestion amount is unable to catch up with the growth of quantity discharged far away, and belongs to low value-added, and the extensive style of low technical content utilizes.On the other hand, containing the abundant useful element such as aluminium, silicon, iron in flyash, wherein dioxide-containing silica 40 ~ 60%, alumina content 17 ~ 50%, iron oxide content 2 ~ 15%, extracts these useful matteies from flyash, becomes the focus of flyash higher value application.And current flyash higher value application mainly concentrates on the extraction aspect of aluminum oxide.
Domestic and international treated coal ash is broadly divided into alkaline process and acid system.In the sixties in last century, Poland just utilizes soda-lime sintering process to extract aluminum oxide from flyash, has built up the pilot plant producing 5000 tons of aluminum oxide and 350,000 tons of cement per year.Institute of Metallurgical Technology of Anhui Province of China and Anhui Cement research institute combine in the eighties has declared by limestone sintering, and sodium carbonate stripping extracts aluminum oxide from flyash, and residue for the production of the achievement of cement, and have passed expert statement.Although alkaline process treated coal ash report is a lot, have no industrialized report at present.Its reason is that alkali process is tediously long, and facility investment is large, and energy consumption is high, cost is high, and the level of residue produced is the several times of flyash, a large amount of cement market goods locally difficulties that residue is made, comprehensive benefit is poor, thus hinders the application of alkaline process in total utilization of PCA.
Compared with alkaline process, acidic process flyash has obvious advantage.Acid system, while effectively extracting aluminum oxide, can obtain silicon product, can be made into white carbon black further and sell after process.Acid technological process facility investment is little, and energy consumption is low, and cost is also low, and level of residue is little, but the conversion unit manufacture used has certain difficulty.Moreover the fine particles that flyash is formed after being through high-temp combustion, wherein glassy phase and corundum have accounted for more than 80%, have had a strong impact on the activity of flyash and acid-respons.Therefore, need to improve flyash with sour reactive behavior to improve the solubility rate of aluminum oxide etc.The more of bibliographical information adds solubility promoter (as NH in Acid leaching reaction
4what CaF of F), but solubility rate is still lower, only has 35 ~ 45%, and resource utilization is low, and with the addition of fluorine element environment being had to pollution, causes secondary pollution.In a word, the higher value application of current flyash only focuses on the extraction of wherein aluminium, and ignores wherein silicon, the extraction of the elements such as iron, is difficult to produce economic benefit.
Summary of the invention
The technical problem to be solved in the present invention is: provide a kind for the treatment of process for circulating fluid bed coal ash, therefrom extract the useful elements such as aluminium, silicon and iron, can also obtain hydrogen chloride gas and ammonia simultaneously, thus realize the comprehensive higher value application of flyash.
Principle of the present invention is: utilize different from acid-respons ability and the different compound of each compound in flyash in the solution that pH value is different, precipitate the difference of character, the metallic compound that will extract is separated from the flyash of complicated component, and purified, this is theoretical foundation of the present invention and basic ideas.
Technical scheme of the present invention is: a kind for the treatment of process for circulating fluid bed coal ash, comprises the following steps:
(1) will come from circulating fluid bed coal ash be ground to after 200 ~ 400 orders with mixed in hydrochloric acid, concentration of hydrochloric acid is 34 ~ 36%, according to 1.8 ~ 2 tons of industrial concentrated hydrochloric acids of the flyash adapted after grinding per ton, be heated to 90 ~ 150 DEG C of reactions 1 ~ 3 hour, and obtain filter residue and leaching liquid after filtering.Filter residue processes further and can obtain white carbon black or material of construction.
(2) adjusting leaching liquid pH value with ammoniacal liquor is 1.5 ~ 3.5, through precipitation, obtains filter residue and filtrate after filtration, and filter residue, through washing, obtains the compound of iron after oven dry.
(3) after carrying iron with ammoniacal liquor adjustment, the pH value of filtrate is 3.8 ~ 5.2, and through precipitation, obtain filter residue and filtrate after filtration, filter residue is through washing, and obtain aluminium hydroxide after oven dry, aluminium hydroxide can obtain metallurgical-grade aluminum oxide in 40 ~ 100 minutes 1050 DEG C of calcinings.
(4) ammonium chloride solution obtained after carrying aluminium is added magnesium oxide and carry out ammonia still process and hydrolysis reaction, the mol ratio of magnesium oxide and ammonium chloride is 0.8 ~ 1:1, and ammonia still process temperature of reaction is 110 ~ 130 DEG C, and hydrolysising reacting temperature is 550 ~ 580 DEG C, be obtained by reacting hydrogen chloride gas, ammonia and magnesium oxide.
Filter residue in described step (2) is dried at 100 DEG C can obtain iron oxide yellow, and iron oxide yellow can obtain red iron oxide 240 ~ 260 DEG C of calcinations.
The magnesium oxide of reaction gained in described step (4), and hydrogen chloride gas, ammonia all can turn back to recycle in step (1) to step (4) after absorbing.
Four described steps form the complete comprehensive higher value application technique of flyash; Meanwhile, wherein any one step in four steps is added together with the content be associated in other step, also forms four and is mutually related again independently of one another, and be the complete comprehensive higher value application technique of flyash.
According to technique of the present invention, white carbon black can be extracted from circulating fluid bed coal ash, iron oxide yellow, red iron oxide, the many kinds of substances such as metallurgical-grade aluminum oxide.Various product has been widely used, as red iron oxide can be used as rubber, and paint, the tinting material of plastics etc., iron oxide yellow can be used as pigment, the catalyzer of rust-inhibiting paint and organic synthesis, waste water conditioners etc., aluminum oxide can be used as the basic raw material of electrolytic aluminum, and then can produce various aluminiums etc.Through chemical examination, every product purity is high, and all technical all meets national relevant technologies specification of quality.(silicon oxide-containing 50% in flyash is supposed by China's circulating fluid bed coal ash annual emissions 0.2 hundred million tons, aluminum oxide 30%, ferric oxide 2%), the rate of recovery gets 70%, metallurgical-grade aluminum oxide 0.04 hundred million ton can be produced, red iron oxide 0.003 hundred million ton, white carbon black 0.07 hundred million ton, annual value of production is up to 443.2 hundred million yuan, and economic benefit is very considerable.And of the present invention simple for process, reasonable in design, required equipment is also fairly simple, invests little.The comprehensive higher value application technique of flyash of the present invention effectively overcomes the problem of environmental pollution of flyash, substantially reduces the harm of flyash.
Ammonia still process is carried out and hydrolysis reaction principle is: join in ammonium chloride solution by magnesium oxide with magnesium oxide, under 105 ~ 135 DEG C of boilings, reaction steams ammonia, and obtain magnesium chloride solution, this solution is heated to 500 ~ 600 DEG C, there is the hydrolysis of magnesium chloride, obtain hydrogen chloride gas and magnesium oxide, gas all can Returning process recycle with magnesium oxide after absorbing.Involved chemical reaction has:
Ammonia still process is reacted: MgO+2NH
4cl=2NH
3+ H
2o+MgCl
2
Hydrolysis reaction: MgCl
2+ H
2o=MgO+2HCl
Compared with the method for other treated coal ash, advantage of the present invention has:
(1) the present invention adopts simple chemical precipitation method, and extracted by the useful elements such as the silicon in flyash, aluminium, iron, high financial profit, achieves the comprehensive higher value application of flyash.
(2) present invention process can extract white carbon black from flyash, iron oxide yellow, red iron oxide, the multiple products such as aluminum oxide, and various product has been widely used, and added value of product is high.
(3) hydrochloric acid in the present invention, magnesium oxide and ammoniacal liquor all can realize recycle, three-waste free pollution, and what achieve flyash cleans utilization.
(4) technological process of the present invention is simple, and invest little, cost is low, and added value of product is high, is a circulating fluid bed coal ash method of comprehensive utilization having industrialization prospect.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Embodiment
Embodiment 1
(1) somewhere circulating fluid bed coal ash (chemical group prejudice table 1) is ground to 200 orders.Get 1 kilogram, the flyash after grinding to mix with the concentrated hydrochloric acid that 1.8 kilogram-mass marks are about 35%, reaction 1.5 hours, and obtain filter residue and leaching liquid after filtering.Filter residue, through water counter flow washing, obtains white carbon black after process further, knows that the extraction yield of silicon is 97% as calculated.
(2) adjusting leaching liquid pH value with ammoniacal liquor is 3.2, filter with filter precipitate 3 hours at 50 DEG C after, obtain filter residue and filtrate, filter residue is through water washing, iron oxide yellow is obtained after drying at 100 DEG C, iron oxide yellow obtains red iron oxide 260 DEG C of calcinations, knows that the extraction yield of iron is 78% as calculated.
(3) after carrying iron with ammoniacal liquor adjustment, filtrate pH value is 5.1, filter with filter precipitate 3 hours at 50 DEG C after, obtain filter residue and filtrate, filter residue is through water washing, aluminium hydroxide is obtained after oven dry, aluminium hydroxide obtains metallurgical-grade aluminum oxide 1050 DEG C of calcinings after 50 minutes, knows that the extraction yield of aluminium is 80% as calculated
(4) add magnesium oxide by carrying the filtrate after aluminium, the mol ratio of magnesium oxide and ammonium chloride is 0.8:1, ammonia still process temperature of reaction 125 DEG C, hydrolysising reacting temperature 550 DEG C, the hydrogen chloride gas obtain recovery and ammonia measure, and the rate of recovery of known ammonia is 92%, the hydrogen chloride gas rate of recovery 91%.
Table 1 circulating fluid bed coal ash chemical constitution
| Composition | Al 2O 3 | SiO 2 | Fe 2O 3 | CaO | TiO 2 | K 2O | Na 2O | MgO | Burn alkali | Other | Amount to |
| % | 48.20 | 38.33 | 1.85 | 3.42 | 1.1 | 0.33 | 0.21 | 0.09 | 5.21 | 1.26 | 100.00 |
Embodiment 2
(1) somewhere circulating fluid bed coal ash as shown in table 1 for chemical constitution is ground to 250 orders.Get 1 kilogram, the flyash after grinding to mix with the concentrated hydrochloric acid that 1.5 kilogram-mass marks are about 34%, 100 DEG C of reactions 1 hour, and obtain filter residue and leaching liquid after filtering.Filter residue, through water counter flow washing, obtains white carbon black after process further, knows that the extraction yield of silicon is 96% as calculated.
(2) adjusting leaching liquid pH value with ammoniacal liquor is 2.2, filters, obtain filter residue and filtrate at 50 DEG C after precipitating 3 hours with filter, filter residue is through washing, obtain iron oxide yellow after drying at 100 DEG C, iron oxide yellow obtains red iron oxide 260 DEG C of calcinations, knows that the extraction yield of iron is 55% as calculated.
(3) after carrying iron with ammoniacal liquor adjustment, filtrate pH value is 4.4, filter with filter precipitate 3 hours at 50 DEG C after, obtain filter residue and filtrate, filter residue is through washing, aluminium hydroxide is obtained after oven dry, aluminium hydroxide obtains metallurgical-grade aluminum oxide 1050 DEG C of calcinings after 50 minutes, knows that the extraction yield of aluminium is 61% as calculated.
(4) add magnesium oxide by carrying the filtrate after aluminium, the mol ratio of magnesium oxide and ammonium chloride is 0.5:1, ammonia still process temperature of reaction 110 DEG C, hydrolysising reacting temperature 520 DEG C, the hydrogen chloride gas obtain recovery and ammonia measure, and the rate of recovery of known ammonia is 82%, the hydrogen chloride gas rate of recovery 88%.
Embodiment 3
(1) somewhere circulating fluid bed coal ash as shown in table 1 for chemical constitution is ground to 300 orders.Get 1 kilogram, the flyash after grinding to mix with the concentrated hydrochloric acid that 2 kilogram-mass marks are about 36%, 150 DEG C of reactions 3 hours, and obtain filter residue and leaching liquid after filtering.Filter residue, through water counter flow washing, obtains white carbon black after process further, knows that the extraction yield of silicon is 97% as calculated.
(2) adjusting leaching liquid pH value with ammoniacal liquor is 3.5, filters, obtain filter residue and filtrate at 50 DEG C after precipitating 3 hours with filter, filter residue is through washing, obtain iron oxide yellow after drying at 100 DEG C, iron oxide yellow obtains red iron oxide 260 DEG C of calcinations, knows that the extraction yield of iron is 81% as calculated.
(3) after carrying iron with ammoniacal liquor adjustment, filtrate pH value is for being 5.1, filter with filter precipitate 3 hours at 50 DEG C after, obtain filter residue and filtrate, filter residue is through washing, aluminium hydroxide is obtained after oven dry, aluminium hydroxide obtains metallurgical-grade aluminum oxide 1050 DEG C of calcinings after 50 minutes, knows that the extraction yield of aluminium is 83% as calculated.
(4) add magnesium oxide by carrying the filtrate after aluminium, the mol ratio of magnesium oxide and ammonium chloride is 1:1, ammonia still process temperature of reaction 130 DEG C, hydrolysising reacting temperature 580 DEG C, the hydrogen chloride gas obtain recovery and ammonia measure, and the rate of recovery of known ammonia is 92%, the hydrogen chloride gas rate of recovery 94%.
Embodiment 4
(1) somewhere circulating fluid bed coal ash as shown in table 1 for chemical constitution is ground to 400 orders.Get 1 kilogram, the flyash after grinding to mix with the concentrated hydrochloric acid that 1.6 kilogram-mass marks are about 34%, 120 DEG C of reactions 2 hours, and obtain filter residue and leaching liquid after filtering.Filter residue, through water counter flow washing, obtains white carbon black after process further, knows that the extraction yield of silicon is 95% as calculated.
(2) adjusting leaching liquid pH value with ammoniacal liquor is 3.0, filters, obtain filter residue and filtrate at 50 DEG C after precipitating 3 hours with filter, filter residue is through washing, obtain iron oxide yellow after drying at 100 DEG C, iron oxide yellow obtains red iron oxide 260 DEG C of calcinations, knows that the extraction yield of iron is 76% as calculated.
(3) after carrying iron with ammoniacal liquor adjustment, filtrate pH value is 4.8 precipitate after 3 hours at 50 DEG C and filter with filter, obtain filter residue and filtrate, filter residue is through washing, aluminium hydroxide is obtained after oven dry, aluminium hydroxide obtains metallurgical-grade aluminum oxide 1050 DEG C of calcinings after 50 minutes, knows that the extraction yield of aluminium is 78% as calculated.
(4) add magnesium oxide by carrying the filtrate after aluminium, the mol ratio of magnesium oxide and ammonium chloride is 0.6:1, ammonia still process temperature of reaction 120 DEG C, hydrolysising reacting temperature 560 DEG C, the hydrogen chloride gas obtain recovery and ammonia measure, and the rate of recovery of known ammonia is 85%, the hydrogen chloride gas rate of recovery 87%.
Claims (4)
1. for a treatment process for circulating fluid bed coal ash, it is characterized in that, comprise the following steps:
(1) will come from circulating fluid bed coal ash be ground to after 200 ~ 400 orders with mixed in hydrochloric acid, hydrochloric acid is the concentrated hydrochloric acid of 30% ~ 36%, hydrochloric acid adapted ratio is flyash adapted 1.8 ~ 2 tons of concentrated hydrochloric acids after grinding per ton, be heated to 90 ~ 150 DEG C of reactions 1 ~ 3 hour, and obtain filter residue and leaching liquid after filtering;
(2) adjusting leaching liquid pH value with ammoniacal liquor is 1.5 ~ 3.5, after precipitation, filtration, obtain filter residue and filtrate, and filter residue obtains the compound of iron after washing, oven dry;
(3) after carrying iron with ammoniacal liquor adjustment, the pH value of filtrate is 3.8 ~ 5.2, and through precipitation, obtain filter residue and filtrate after filtration, filter residue, through washing, obtains aluminium hydroxide after oven dry, aluminium hydroxide is obtained metallurgical-grade aluminum oxide in 20 ~ 120 minutes 900 ~ 1100 DEG C of calcinings;
(4) ammonium chloride solution obtained after carrying aluminium is added magnesium oxide and carry out ammonia still process and hydrolysis reaction, the mol ratio of magnesium oxide and ammonium chloride is 0.5 ~ 1:1, ammonia still process temperature of reaction is 105 ~ 135 DEG C, and hydrolysising reacting temperature is 500 ~ 600 DEG C, is obtained by reacting hydrogen chloride gas, ammonia and magnesium oxide.
2. a kind for the treatment of process for circulating fluid bed coal ash according to claim 1, is characterized in that: the filter residue in step (2) is dried and obtained iron oxide yellow at 100 DEG C.
3. a kind for the treatment of process for circulating fluid bed coal ash according to claim 2, is characterized in that: iron oxide yellow obtains red iron oxide 200 ~ 300 DEG C of calcinations.
4. a kind for the treatment of process for circulating fluid bed coal ash according to claim 1, is characterized in that: the magnesium oxide produced in step (4), and hydrogen chloride gas after absorbing and ammonia return recycle in step (1) to step (4).
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