CN104445212B - A kind of processing method for circulating fluid bed coal ash - Google Patents
A kind of processing method for circulating fluid bed coal ash Download PDFInfo
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- CN104445212B CN104445212B CN201310420532.6A CN201310420532A CN104445212B CN 104445212 B CN104445212 B CN 104445212B CN 201310420532 A CN201310420532 A CN 201310420532A CN 104445212 B CN104445212 B CN 104445212B
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Abstract
The present invention relates to a kind of processing method for circulating fluid bed coal ash, including circulating fluid bed coal ash will be come from through hydrochloric acid dissolution, filter residue and leaching liquid are obtained after filtering；It is 1.5~3.5 with ammoniacal liquor adjustment leaching liquid pH value, through precipitation, filter residue and filtrate is obtained after filtering, filter residue is scrubbed, the compound of iron is obtained after drying；It is 3.8~5.2 to put forward the filtrate pH value after iron with ammoniacal liquor adjustment, through precipitation, filter residue and filtrate is obtained after filtering, filter residue is scrubbed, and aluminium hydroxide is obtained after drying, further obtains metallurgical-grade aluminum oxide after calcining；The ammonium chloride solution addition magnesia progress ammonia still process obtained after aluminium and hydrolysis will be carried, obtain hydrogen chloride gas, ammonia and magnesia.The step by step arithmetic of the useful element such as aluminium, silicon, iron in the achievable flyash of the present invention, while material of the present invention can be achieved to recycle, technical process is simple and direct, and cost is low, is that circulating fluid bed coal ash higher value application opens new approach.
Description
Technical field
It is more particularly to a kind of to utilize step-by-step precipitation method from recirculating fluidized bed the invention belongs to flyash higher value application field
The method that the useful elements such as aluminium, silicon and iron are extracted in flyash.
Background technology
In recent years, solid waste coal ash discharge capacity is brought while the coal electricity industry of China is developed rapidly drastically
Increase, by 2007, the annual emissions of China's flyash were still increasing year by year more than 200,000,000 tons, added up volume of cargo in storage more than 25
Hundred million tons.The flyash largely discharged had both taken a large amount of soils, and caused severe contamination to soil, water resource and air.Therefore, powder
The comprehensive utilization of coal ash turns into the task of top priority.
At present, flyash is building work, and the multiple fields such as building are applied, although large usage quantity, its digestion amount is remote
Far the growth of discharge capacity is unable to catch up with, and belong to low value-added, the extensive style of low technical content is utilized.On the other hand, in flyash
Contain the useful elements such as abundant aluminium, silicon, iron, wherein dioxide-containing silica 40~60%, alumina content 17~50%, iron oxide
Content 2~15%, extracts these utilities from flyash, the focus as flyash higher value application.And it is current
In terms of flyash higher value application is concentrated mainly on the extraction of aluminum oxide.
Domestic and international treated coal ash is broadly divided into alkaline process and acid system.The sixties in last century, Poland just utilizes soda lime
Sintering process extracts aluminum oxide from flyash, has built up the pilot plant for producing 5000 tons of aluminum oxide and 350,000 tons of cement per year.China
Institute of Metallurgical Technology of Anhui Province and Anhui Cement research institute combine in the eighties has declared by limestone sintering, sodium carbonate dissolution from
Aluminum oxide is extracted in flyash, residue is used for the achievement for producing cement, and has passed through expert appraisal.Although alkaline process treated coal ash
Report is a lot, but has no industrialized report at present.Its reason is that alkali process is tediously long, and equipment investment is big, high energy consumption, cost
Height, and the level of residue produced is the several times of flyash, and a large amount of cement market goods locallies that residue is made are difficult, and comprehensive benefit is poor,
Thus hinder application of the alkaline process in terms of total utilization of PCA.
Compared with alkaline process, acid treatment flyash has obvious advantage.Acid system, can be with while aluminum oxide is effectively extracted
Silicon product is obtained, further white carbon is can be made into after processing and sells.Acid technological process equipment investment is small, and energy consumption is low, and cost is also low,
Level of residue is small, but the consersion unit manufacture used has certain difficulty.Furthermore, flyash is formed after high-temp combustion thin
Little particulate, wherein glass phase have accounted for more than 80% with corundum, have had a strong impact on the activity of flyash and acid reaction.Accordingly, it would be desirable to
Improve flyash with the reactivity of acid to improve the dissolution rate of aluminum oxide etc..The more of document report is in Acid leaching reaction
Middle addition cosolvent（Such as NH4What CaF of F）, but dissolution rate is still than relatively low, and only 35~45%, resource utilization is low, and addition
There is to environment the fluorine element of pollution, cause secondary pollution.In a word, the higher value application of current flyash only focuses on wherein aluminium
Extraction, and ignore wherein silicon, the extraction of the element such as iron, it is difficult to produce economic benefit.
The content of the invention
The technical problem to be solved in the present invention is：A kind of processing method for circulating fluid bed coal ash is provided, therefrom
The useful elements such as aluminium, silicon and iron are extracted, while hydrogen chloride gas and ammonia can also be obtained, so that it is high-valued to realize that flyash is integrated
Utilize.
The present invention principle be：It is different from acid reaction ability and different compounds are in pH using each compound in flyash
The difference of property is precipitated in the different solution of value, the metallic compound to be extracted is isolated from the flyash of complicated component
Come, and purified, this is the theoretical foundation and basic ideas of the present invention.
The technical scheme is that：A kind of processing method for circulating fluid bed coal ash, comprises the following steps：
（1）To come from circulating fluid bed coal ash be ground to after 200~400 mesh with mixed in hydrochloric acid, concentration of hydrochloric acid is 34
~36%, according to the industrial concentrated hydrochloric acid of 1.8~2 tons of flyash adapted after grinding per ton, it is heated to 90~150 DEG C of reactions 1~3 small
When, and obtain filter residue and leaching liquid after filtering.Further processing can obtain white carbon or construction material to filter residue.
（2）It is 1.5~3.5 with ammoniacal liquor adjustment leaching liquid pH value, through precipitation, filter residue and filtrate, filter residue warp is obtained after filtering
Washing, obtains the compound of iron after drying.
（3）It is 3.8~5.2 to be adjusted with ammoniacal liquor and put forward the pH value of filtrate after iron, and through precipitation, filter residue and filtrate are obtained after filtering,
Filter residue is scrubbed, and aluminium hydroxide is obtained after drying, and aluminium hydroxide can obtain metallurgical grade oxygen in 40~100 minutes in 1050 DEG C of calcinings
Change aluminium.
（4）The ammonium chloride solution addition magnesia progress ammonia still process and hydrolysis, magnesia and chlorination obtained after aluminium will be proposed
The mol ratio of ammonium is 0.8~1:1, ammonia still process reaction temperature is 110~130 DEG C, and hydrolysising reacting temperature is 550~580 DEG C, is reacted
To hydrogen chloride gas, ammonia and magnesia,.
Described step（2）In filter residue dried at 100 DEG C and can obtain iron oxide yellow, and iron oxide yellow is 240~260
DEG C calcination can obtain iron oxide red.
Described step（4）Magnesia obtained by middle reaction, and hydrogen chloride gas, ammonia can return to after absorption
Step（1）To step（4）In recycle.
Four described steps constitute a complete flyash and integrate higher value application technique；Meanwhile, in four steps
One step content associated with other steps of any of which be added together, also constitute four independently of one another and mutually close
Connection, and be that complete flyash integrates higher value application technique.
According to technique of the present invention, white carbon, iron oxide yellow, iron oxide can be extracted from circulating fluid bed coal ash
It is red, many kinds of substance such as metallurgical-grade aluminum oxide.Various products have been widely used, as iron oxide red can be painted, plastics as rubber
Deng colouring agent, iron oxide yellow can be as pigment, the catalyst of antirust paint and organic synthesis, waste water treating agent etc., and aluminum oxide can
As the basic raw material of electrolytic aluminium, and then various aluminiums etc. can be produced.Through chemical examination, every product purity is high, and every technology refers to
Mark meets the relevant technical quality requirement of country.Based on 0.2 hundred million tons of China's circulating fluid bed coal ash annual emissions（Assuming that fine coal
Silicon oxide-containing 50% in ash, aluminum oxide 30%, iron oxide 2%）, the rate of recovery takes 70%, can produce 0.04 hundred million tons of metallurgical-grade aluminum oxide,
0.003 hundred million tons of iron oxide red, 0.07 hundred million tons of white carbon, annual value of production is up to 443.2 hundred million yuan, and economic benefit is very considerable.And this
That invents is simple for process, and reasonable in design, required equipment is also fairly simple, invests small.The flyash of the present invention integrates high level
Change the problem of environmental pollution that flyash is effectively overcomed using technique, substantially reduce the harm of flyash.
Ammonia still process and hydrolysis principle are carried out with magnesia is：Magnesia is added in ammonium chloride solution, 105~
The lower reaction of 135 DEG C of boilings steams ammonia, and obtains magnesium chloride solution, and the solution is heated into 500~600 DEG C, occurs magnesium chloride
Hydrolysis, obtain hydrogen chloride gas and magnesia, gas can return to flow with magnesia after absorption and recycle.It is involved
Chemical reaction have：
Ammonia still process is reacted：MgO+2NH4Cl=2NH3+H2O+MgCl2
Hydrolysis：MgCl2+H2O=MgO+2HCl
Compared with the method for other treated coal ashs, advantages of the present invention has：
（1）The present invention uses simple chemical precipitation method, and the useful elements such as the silicon in flyash, aluminium, iron are extracted
Come, high financial profit realizes the synthesis higher value application of flyash.
（2）Present invention process can extract white carbon from flyash, iron oxide yellow, iron oxide red, a variety of productions such as aluminum oxide
Product, various products have been widely used, and added value of product is high.
（3）Hydrochloric acid, magnesia and ammoniacal liquor in the present invention can be achieved to recycle, and three-waste free pollution realizes fine coal
Grey cleans utilization.
（4）The technical process of the present invention is simple, invests small, cost is low, added value of product is high, is one and has industrialization
The circulating fluid bed coal ash method of comprehensive utilization of prospect.
Brief description of the drawings
Fig. 1 is process flow diagram of the invention.
Embodiment
Embodiment 1
（1）By somewhere circulating fluid bed coal ash（Chemical composition is shown in Table 1）It is ground to 200 mesh.Take the flyash 1 after grinding
Kilogram concentrated hydrochloric acid for being about 35% with 1.8 kilogram-mass fractions was mixed, in reaction 1.5 hours, and obtained filter residue and leaching after filtering
Liquid.Filter residue further obtains white carbon through water counter flow washing after processing, and the recovery rate for being computed knowing silicon is 97%.
（2）It is 3.2 with ammoniacal liquor adjustment leaching liquid pH value, is filtered, obtained with filter after being precipitated 3 hours at 50 DEG C
Filter residue and filtrate, filter residue obtain iron oxide yellow, iron oxide yellow obtains oxygen in 260 DEG C of calcinations through water washing after being dried at 100 DEG C
Change iron oxide red, the recovery rate for being computed knowing iron is 78%.
（3）It is 5.1 to put forward filtrate pH value after iron with ammoniacal liquor adjustment, is filtered after being precipitated 3 hours at 50 DEG C with filter,
Filter residue and filtrate are obtained, filter residue obtains aluminium hydroxide through water washing after drying, aluminium hydroxide is obtained after being calcined 50 minutes at 1050 DEG C
To metallurgical-grade aluminum oxide, the recovery rate for being computed knowing aluminium is 80%
（4）The addition magnesia of the filtrate after aluminium will be carried, the mol ratio of magnesia and ammonium chloride is 0.8:1, ammonia still process reaction temperature
125 DEG C of degree, 550 DEG C of hydrolysising reacting temperature, the hydrogen chloride gas that recovery is obtained is measured with ammonia, it is known that the rate of recovery of ammonia
For 92%, the hydrogen chloride gas rate of recovery 91%.
The circulating fluid bed coal ash chemical composition of table 1
| Composition | Al2O3 | SiO2 | Fe2O3 | CaO | TiO2 | K2O | Na2O | 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）Chemical composition somewhere circulating fluid bed coal ash as shown in table 1 is ground to 250 mesh.Take the powder after grinding
The concentrated hydrochloric acid that 1 kilogram of coal ash is about 34% with 1.5 kilogram-mass fractions is mixed, and is reacted 1 hour at 100 DEG C, and is filtered after filtering
Slag and leaching liquid.Filter residue further obtains white carbon through water counter flow washing after processing, and the recovery rate for being computed knowing silicon is 96%.
（2）It is 2.2 with ammoniacal liquor adjustment leaching liquid pH value, is filtered, obtained with filter after being precipitated 3 hours at 50 DEG C
Filter residue and filtrate, filter residue are scrubbed, obtain iron oxide yellow after being dried at 100 DEG C, iron oxide yellow is aoxidized in 260 DEG C of calcinations
Iron oxide red, the recovery rate for being computed knowing iron is 55%.
（3）It is 4.4 to put forward filtrate pH value after iron with ammoniacal liquor adjustment, is filtered after being precipitated 3 hours at 50 DEG C with filter,
Filter residue and filtrate are obtained, filter residue is scrubbed, aluminium hydroxide is obtained after drying, aluminium hydroxide is obtained after being calcined 50 minutes at 1050 DEG C
Metallurgical-grade aluminum oxide, the recovery rate for being computed knowing aluminium is 61%.
（4）The addition magnesia of the filtrate after aluminium will be carried, the mol ratio of magnesia and ammonium chloride is 0.5:1, ammonia still process reaction temperature
110 DEG C of degree, 520 DEG C of hydrolysising reacting temperature, the hydrogen chloride gas that recovery is obtained is measured with ammonia, it is known that the rate of recovery of ammonia
For 82%, the hydrogen chloride gas rate of recovery 88%.
Embodiment 3
（1）Chemical composition somewhere circulating fluid bed coal ash as shown in table 1 is ground to 300 mesh.Take the powder after grinding
The concentrated hydrochloric acid that 1 kilogram of coal ash is about 36% with 2 kilogram-mass fractions is mixed, and is reacted 3 hours at 150 DEG C, and obtains filter residue after filtering
With leaching liquid.Filter residue further obtains white carbon through water counter flow washing after processing, and the recovery rate for being computed knowing silicon is 97%.
（2）It is 3.5 with ammoniacal liquor adjustment leaching liquid pH value, is filtered, obtained with filter after being precipitated 3 hours at 50 DEG C
Filter residue and filtrate, filter residue are scrubbed, obtain iron oxide yellow after being dried at 100 DEG C, iron oxide yellow is aoxidized in 260 DEG C of calcinations
Iron oxide red, the recovery rate for being computed knowing iron is 81%.
（3）It is 5.1 to put forward filtrate pH value after iron with ammoniacal liquor adjustment, is carried out after being precipitated 3 hours at 50 DEG C with filter
Filter, obtains filter residue and filtrate, filter residue is scrubbed, aluminium hydroxide is obtained after drying, aluminium hydroxide is after 1050 DEG C are calcined 50 minutes
Metallurgical-grade aluminum oxide is obtained, the recovery rate for being computed knowing aluminium is 83%.
（4）The addition magnesia of the filtrate after aluminium will be carried, the mol ratio of magnesia and ammonium chloride is 1:1, ammonia still process reaction temperature
130 DEG C, 580 DEG C of hydrolysising reacting temperature will reclaim obtained hydrogen chloride gas and be measured with ammonia, it is known that the rate of recovery of ammonia is
92%, the hydrogen chloride gas rate of recovery 94%.
Embodiment 4
（1）Chemical composition somewhere circulating fluid bed coal ash as shown in table 1 is ground to 400 mesh.Take the powder after grinding
The concentrated hydrochloric acid that 1 kilogram of coal ash is about 34% with 1.6 kilogram-mass fractions is mixed, and is reacted 2 hours at 120 DEG C, and is filtered after filtering
Slag and leaching liquid.Filter residue further obtains white carbon through water counter flow washing after processing, and the recovery rate for being computed knowing silicon is 95%.
（2）It is 3.0 with ammoniacal liquor adjustment leaching liquid pH value, is filtered, obtained with filter after being precipitated 3 hours at 50 DEG C
Filter residue and filtrate, filter residue are scrubbed, obtain iron oxide yellow after being dried at 100 DEG C, iron oxide yellow is aoxidized in 260 DEG C of calcinations
Iron oxide red, the recovery rate for being computed knowing iron is 76%.
（3）Carried after filtrate pH value is precipitated 3 hours for 4.8 at 50 DEG C after iron and being filtered with filter with ammoniacal liquor adjustment,
Filter residue and filtrate are obtained, filter residue is scrubbed, aluminium hydroxide is obtained after drying, aluminium hydroxide is obtained after being calcined 50 minutes at 1050 DEG C
Metallurgical-grade aluminum oxide, the recovery rate for being computed knowing aluminium is 78%.
（4）The addition magnesia of the filtrate after aluminium will be carried, the mol ratio of magnesia and ammonium chloride is 0.6:1, ammonia still process reaction temperature
120 DEG C of degree, 560 DEG C of hydrolysising reacting temperature, the hydrogen chloride gas that recovery is obtained is measured with ammonia, it is known that the rate of recovery of ammonia
For 85%, the hydrogen chloride gas rate of recovery 87%.
Claims (1)
1. a kind of processing method for circulating fluid bed coal ash, it is characterised in that comprise the following steps：
（1）To come from circulating fluid bed coal ash be ground to after 200~400 mesh with mixed in hydrochloric acid, hydrochloric acid is 30%~36%
Concentrated hydrochloric acid, hydrochloric acid adapted ratio is 1.8~2 tons of concentrated hydrochloric acids of flyash adapted after grinding per ton, is heated to 90~150 DEG C of reactions
Filter residue and leaching liquid are obtained behind 1~3 hour, and filtering；
（2）It is 1.5~3.5 with ammoniacal liquor adjustment leaching liquid pH value, obtains filter residue and filtrate after precipitation, filtering, filter residue is scrubbed,
The compound of iron is obtained after drying；
（3）It is 3.8~5.2 to be adjusted with ammoniacal liquor and put forward the pH value of filtrate after iron, and through precipitation, filter residue and filtrate, filter residue are obtained after filtering
It is scrubbed, aluminium hydroxide is obtained after drying, aluminium hydroxide is obtained into metallurgical grade oxygen in 20~120 minutes in 900~1100 DEG C of calcinings
Change aluminium；
（4）The ammonium chloride solution addition magnesia obtained after aluminium will be carried and carry out ammonia still process and hydrolysis, magnesia and ammonium chloride
Mol ratio is 0.5~1:1, ammonia still process reaction temperature is 105~135 DEG C, and hydrolysising reacting temperature is 500~600 DEG C, and reaction obtains chlorine
Change hydrogen, ammonia and magnesia；
Step（4）The magnesia of middle generation, and hydrogen chloride gas and ammonia return to step after absorption（1）To step（4）
In recycle；Step（2）In filter residue dried at 100 DEG C and obtain iron oxide yellow；Iron oxide yellow is in 200~300 DEG C of calcinations
Obtain iron oxide red.
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| CN103193238A (en) * | 2013-04-19 | 2013-07-10 | 宫毅 | Method for producing superfine white carbon black, ferric hydroxide and aluminum oxide by using coal ash |
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