CN1792802A - Process for extracting aluminium hydroxide from flyash - Google Patents
Process for extracting aluminium hydroxide from flyash Download PDFInfo
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- CN1792802A CN1792802A CN 200510048274 CN200510048274A CN1792802A CN 1792802 A CN1792802 A CN 1792802A CN 200510048274 CN200510048274 CN 200510048274 CN 200510048274 A CN200510048274 A CN 200510048274A CN 1792802 A CN1792802 A CN 1792802A
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- flyash
- extracting
- aluminium
- filter residue
- alumina
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Abstract
A process for extracting aluminum oxide from powdered coal ash includes such steps as grinding, calcining, mixing with H2SO4 solution, heating while reaction for extracting aluminum oxide, boiling in water, concentrating, cooling while educing out aluminum sulfate crystals, heating for dewatering, heating for decomposing to obtain gamma-Al2O3, and further preparing metallurgy-class aluminum oxide.
Description
Affiliated technical field
The invention belongs to the comprehensive utilization that becomes more meticulous of flyash, specifically relate to a kind of method of alumina of from flyash, extracting.
Background technology
A large amount of flyash of coal-burning power plant's discharging have caused serious pollution to agricultural production and living environment on every side, and comprehensive regulation flyash has become the environmental problem that an exigence solves.In China, the flyash amount of the annual discharging in coal-burning power plant is up to more than one hundred million tons, and volume of cargo in storage is very big.Al in the flyash
2O
3Content is higher, is about 20~40%, because volume of cargo in storage is big, is one and has the resource treasure-house that the comprehensive development and utilization that becomes more meticulous is worth.
From flyash, extract Al both at home and abroad
2O
3Method can be divided into alkaline process and acid system two big classes.In the sixties in last century, Poland just utilizes soda lime sintering process to extract Al in flyash
2O
3, built up and produced 5000 tons of Al per year
2O
3And the pilot plant of 350,000 tons of cement.China Anhui Province Institute of Metallurgical Technology and Hefei cement research institute have declared with limestone sintering, sodium carbonate stripping in the eighties and extracted Al in flyash
2O
3, residue is for the production of the achievement of cement, in March nineteen eighty-two by expert appraisal.The soda lime sintering process of building materials research institute of Ningxia autonomous region research extracts Al in flyash
2O
3, residue produce cement industry in September, 1987 by the Ningxia State Scientific and Technological Commission of autonomous region tissue characterization.In December, 2004, Inner Mongolia Autonomous Region Science and Technology Department has held " flyash extracts the aluminum and coproducing cement industrialization technology " the project appraisal of scientific and technological achievements meeting of covering the research and development of western new and high technology Group Co.,Ltd, and this group has independently finished nearly 5000 tonnes pilot scale.Although extract Al about alkaline process
2O
3Report a lot, adopt above-mentioned process half industrialization and industrialization quantity-produced report but have not yet to see.Its reason is to handle the numerous length of technology that this high silicon contains the aluminium powder coal ash with alkaline process, the inventory of running is big, facility investment is also big, the energy consumption height, the cost height, and also the level of residue that produces is the several times of flyash amount, limited with a large amount of cement market goods locallies that residue is made, overall economic efficiency is poor, and level of comprehensive utilization is low, thereby has hindered the application of alkaline process aspect comprehensive utilization flyash.
Compare with alkaline process, come treated coal ash just to have obvious advantage with acid system.Acid system when the aluminum oxide that effectively extracts in the flyash, silica all can be refused outside liquid, can not produce new solid material in process of production, level of residue is little, thereby the inventory of running is little, equipment investment is little, energy consumption is low, product cost is also low.But the shortcoming of acid system is in leaching during aluminum oxide, has also brought into solution such as the many leachable impurity in the flyash such as iron, titanium, magnesium, must increase the postorder treatment process; The conversion unit manufacturing of Shi Yonging has certain degree of difficulty besides.But compare with alkaline process, use still the most promising method of acid treatment fly ash, therefore, the research of carrying out this respect both at home and abroad is more.
Extract aluminium oxide with acid treatment flyash and mostly adopt sulfuric acid or saline and alkaline technology.Because flyash is the tiny grit that forms through after high temperature (1500 ℃) burning, the glassy phase in the grit accounts for more than 90%, has had a strong impact on the activity of flyash and acid reaction, therefore, need to improve the reactivity of flyash and acid to improve Al
2O
3Dissolution rate.The more practice of data report is to add cosolvent NH in the acidleach negate is answered
4F and CaF
2, by the complexing Si oxide, make Al thereby reach
2O
3The purpose of stripping.Adopt said method in flyash, to reclaim Al
2O
3, Al
2O
3Dissolution rate all lower, generally only have 35~45%, resource utilization is low, and because having added the fluorine element that environment is had pollution, has brought secondary pollution, has hindered the development and use that become more meticulous of flyash.
Summary of the invention
The purpose of this invention is to provide a kind of method of extracting aluminium oxide from flyash, this method adopts sulfuric acid high temperature to leach aluminium oxide under normal pressure, does not add any cosolvent, the rate of recovery height of aluminium oxide.
The present invention extracts aluminum oxide from flyash concrete grammar comprises:
Flyash is ground to 200~400 orders, in 300~760 ℃ of calcination activations 1~1.5 hour;
Flyash after the roasting and 60%~98% H
2SO
4Weight ratio according to 1: 1~6 is mixed, and is heated to 160~330 ℃ of reactions 1~1.5 hour, filters spent acid is separated with the filter residue that contains reactant;
The water that adds 2.5~5 times of amounts in the filter residue boiled under 65~90 ℃ molten 30~45 minutes, and the stripping reactant removes by filter residue, and filtrate concentrates postcooling, separates out the Tai-Ace S 150 crystallization;
Tai-Ace S 150 heats up to dewater and obtains anhydrous slufuric acid aluminium;
Continue to heat up and make the decomposition of anhydrous slufuric acid aluminium obtain γ-Al
2O
3, and reclaim SO
3Flue gas.
Filtration temperature when wherein, spent acid being separated with the filter residue that contains reactant is selected 100~180 ℃.
The present invention carries out the processing of distinct methods to concentrating the aluminum sulfate crystallization of separating out after the cooling, can produce aluminium salt and the aluminum oxide of many kinds, specifically:
The Tai-Ace S 150 crystallization being no more than dehydration fully under 400 ℃ the temperature, is generated anhydrous slufuric acid aluminium.
In calcining below 900 ℃, aluminum sulfate is decomposed fully in anhydrous slufuric acid aluminium, all generate active strong γ-Al
2O
3
γ-the Al for preparing
2O
3Boil moltenly at 120~190 ℃ of lower NaOH solution with 150g/L~200g/L, make sodium aluminate solution.Owing to the impurity such as iron contained in the aluminium oxide, calcium, magnesium can not be dissolved by alkali, be present in the solid phase, can remove by filter, after the Separation of Solid and Liquid, form the high sodium aluminate solution of purity.Add aluminium hydroxide crystal seed in solution, the sodium aluminate in the solution is separated out with the form crystallization of aluminium hydroxide, the crystalline aluminum hydroxide that obtains can obtain metallurgical-grade aluminum oxide at 1100 ℃ of temperature lower calcinations.
Anhydrous slufuric acid aluminium decomposes preparation γ-Al
2O
3The time SO that produces
3Flue gas directly passes in the spent acid that filters to isolate and produces sulfuric acid, produces the leaching that the sulfuric acid that obtains is used further to aluminium oxide in the flyash, realizes recycling of sulfate system.
The present invention adopts new flyash activating technology, does not use any cosolvent at normal pressure, with sulfuric acid the aluminium oxide in the flyash is effectively leached, and the dissolution rate of aluminium oxide can reach more than 85%.
Any waste water, waste liquid, waste residue and obnoxious flavour are not discharged in all effectively recycles such as the spent acid that produces in the technical process of the present invention, waste water in the whole process.
The present invention adopts different processing methods, the alumina preparation that leaches from flyash can be become aluminium salt and the aluminum oxide of many kinds.
Technological process of the present invention is simple, invests for a short time, and cost is low, and the added value of product height is a flyash that has the prospect comprehensive utilization industrialization method that becomes more meticulous.
Embodiment
Embodiment 1
Get salic 40% flyash 1t, grind to form 300 purpose fine powders, behind the iron removal by magnetic separation,, obtain activatory flyash in 400 ℃ of following roasting 1.5h.
The H of adding 72% in activating fly ash
2SO
44t is warming up to 300 ℃ and leaches reaction 1h, and aluminum oxide is fully leached, and reacting rear material is used further to after the spent acid that filters out reclaims leach operation next time 150 ℃ of solid-liquid separation, recycles.
Add 4t water in solid slag, be warming up to 80 ℃ and boil molten 40min, filter, filter residue washes with water 2 times, the reverse use of washing lotion.
With the filtrate evaporation concentration, return the stripping operation behind the water vapor condensation that steams, separate out the Tai-Ace S 150 crystallization after the concentrated solution cooling, filter, collect solid crystal 2200Kg.The filtrate evaporation concentration is returned the stripping operation behind the water vapor condensation, concentrated solution returns and leaches the use that is mixed of operation and concentrated acid.
The Tai-Ace S 150 solid crystal that obtains is warming up to 350 ℃ of dehydrations gradually, obtains 1500Kg anhydrous slufuric acid aluminium, returns the stripping operation behind the water vapor condensation of generation.
Anhydrous slufuric acid aluminium continues to be warming up to 453 ℃ and begins to decompose, heating direct to 870 ℃ again, and calcining 6h decomposes anhydrous slufuric acid aluminium fully, generates 350Kg γ-Al
2O
3, the SO that calcining produces
3Flue gas is passed in the spent acid for the production of H
2SO
4
γ-Al
2O
3Join in the NaOH solution of 150g/L, be warming up to 150 ℃ and boil moltenly, remove by filter residue, add a small amount of aluminium hydroxide crystal seed in the filtrate, the sodium aluminate in the filtrate is separated out with the form of crystalline aluminum hydroxide, filter, filtrate cycle is used.
The crystalline aluminum hydroxide that obtains is warming up to 1100 ℃ of calcinings obtains the 350Kg metallurgical-grade aluminum oxide.
Embodiment 2
Get salic 40% flyash 1t, grind to form 200 purpose fine powders, behind the iron removal by magnetic separation,, obtain activatory flyash in 600 ℃ of following roasting 1h.
The H of adding 98% in activating fly ash
2SO
42t is warming up to 250 ℃ and leaches reaction 1.5h, and aluminum oxide is fully leached, and reacting rear material is used further to after the spent acid that filters out reclaims leach operation next time 180 ℃ of solid-liquid separation, recycles.
Add 6t water in solid slag, be warming up to 75 ℃ and boil molten 45min, filter, filter residue washes with water 2 times, the reverse use of washing lotion.
With the filtrate evaporation concentration, return the stripping operation behind the water vapor condensation that steams, separate out the Tai-Ace S 150 crystallization after the concentrated solution cooling, filter, collect solid crystal 2200Kg.The filtrate evaporation concentration is returned the stripping operation behind the water vapor condensation, concentrated solution returns and leaches the use that is mixed of operation and concentrated acid.
The Tai-Ace S 150 solid crystal that obtains is warming up to 400 ℃ of dehydrations gradually, obtains 1480Kg anhydrous slufuric acid aluminium, returns the stripping operation behind the water vapor condensation of generation.
Anhydrous slufuric acid aluminium continues to be warming up to 850 ℃, and calcining 8h decomposes anhydrous slufuric acid aluminium fully, generates 350Kg γ-Al
2O
3, the SO that calcining produces
3Flue gas is passed in the spent acid for the production of H
2SO
4
γ-Al
2O
3Join in the NaOH solution of 150g/L, be warming up to 150 ℃ and boil moltenly, remove by filter residue, add a small amount of aluminium hydroxide crystal seed in the filtrate, the sodium aluminate in the filtrate is separated out with the form of crystalline aluminum hydroxide, filter, filtrate cycle is used.
The crystalline aluminum hydroxide that obtains is warming up to 1100 ℃ of calcinings obtains the 350Kg metallurgical-grade aluminum oxide.
Claims (6)
1, a kind of method of alumina of extracting from flyash comprises:
Flyash is ground to 200~400 orders, in 300~760 ℃ of calcination activations 1~1.5 hour;
Flyash after the roasting and 60%~98% H
2SO
4Weight ratio according to 1: 1~6 is mixed, and is heated to 160~330 ℃ of reactions 1~1.5 hour, filters spent acid is separated with the filter residue that contains reactant;
The water that adds 2.5~5 times of amounts in the filter residue boiled under 65~90 ℃ molten 30~45 minutes, and the stripping reactant removes by filter residue, and filtrate evaporation concentration postcooling is separated out the Tai-Ace S 150 crystallization;
The Tai-Ace S 150 crystallization heats up to dewater and obtains anhydrous slufuric acid aluminium;
Continue to heat up and make the decomposition of anhydrous slufuric acid aluminium obtain γ-Al
2O
3, and reclaim SO
3Flue gas.
2, according to the described method of alumina of from flyash, extracting of claim 1, it is characterized in that, spent acid is separated with the filter residue that contains reactant 100~180 ℃ of filtrations.
3, the method for alumina of extracting from flyash according to claim 1 is characterized in that dehydration generates anhydrous slufuric acid aluminium under 400 ℃ the temperature being no more than with the Tai-Ace S 150 crystallization.
4, the method for extracting aluminium oxide from flyash according to claim 1 is characterized in that anhydrous slufuric acid aluminium is prepared γ-Al at the temperature lower calcination that is no more than 900 ℃
2O
3
5, the method for alumina of extracting from flyash according to claim 1 is characterized in that the SO that reclaims
3Flue gas is produced the vitriol oil with sulfuric acid absorption.
6, the method for extracting aluminium oxide from flyash according to claim 1 is characterized in that the γ-Al for preparing
2O
3Can also boil at 120~190 ℃ of lower NaOH solution with 150g/L~200g/L moltenly, make sodium aluminate solution, remove by filter residue after, the adding aluminium hydroxide crystal seed makes solution separate out crystalline aluminum hydroxide, prepares metallurgical-grade aluminum oxide at 1100 ℃ of temperature lower calcinations.
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