CN103936041B - A kind of recoverying and utilizing method containing aluminium Waste Sulfuric Acid - Google Patents

A kind of recoverying and utilizing method containing aluminium Waste Sulfuric Acid Download PDF

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Publication number
CN103936041B
CN103936041B CN201310018061.6A CN201310018061A CN103936041B CN 103936041 B CN103936041 B CN 103936041B CN 201310018061 A CN201310018061 A CN 201310018061A CN 103936041 B CN103936041 B CN 103936041B
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China
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sulfuric acid
waste
aluminium
steel slag
waste sulfuric
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CN103936041A (en
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宿新泰
秦高飞
杨超
王吉德
马凤云
李志娟
钟梅
武荣兰
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Xinjiang University
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Xinjiang University
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Abstract

The invention discloses a kind of recoverying and utilizing method containing aluminium Waste Sulfuric Acid, utilize the waste steel slag process of discharging in steelmaking process containing aluminium Waste Sulfuric Acid, sulfuric acid concentration in spent acid is made to be less than 1%, and the aluminum oxide reclaimed wherein and ferric oxide, the combined recovery belonged to containing aluminium spent acid and solid waste utilizes technical field.First the method utilizes Rotary Evaporators process containing aluminium Waste Sulfuric Acid, makes sulfuric acid concentration be greater than 70%; With certain solid-liquid ratio waste steel slag joined concentrated after containing in aluminium Waste Sulfuric Acid; Service temperature is 50-100 DEG C, and the reaction times is 1-3h; The hydrogen recovery produced in reaction, for providing thermal source for reaction; Solid-liquid separation, associating removal of impurities, crystallization, calcining, obtain aluminum oxide and ferric oxide solid; The filter residue of solid-liquid separation can be doped in waste steel slag, and doping ratio is 1-10:1(waste steel slag: filter residue), realize recycle.The present invention utilizes the waste steel slag process of discharging in steelmaking process containing aluminium Waste Sulfuric Acid, and the treatment of wastes with processes of wastes against one another, achieves combined governance and the resource reclaim of liquid-solid waste.

Description

A kind of recoverying and utilizing method containing aluminium Waste Sulfuric Acid
Technical field
The invention belongs to a kind of recoverying and utilizing method containing aluminium Waste Sulfuric Acid, the combined recovery particularly containing aluminium Waste Sulfuric Acid and solid waste utilizes technical field.
Background technology
The industry such as automobile, household electrical appliances, aviation, mechanical means, plating, metallurgy uses Al and Alalloy foundry goods as starting material in a large number.These aluminium castings often need to utilize the vitriol oil to carry out flooding and rinsing before using.The sulfuric acid concentration of this Waste Sulfuric Acid washing lotion is 1-20%, and aluminium composition is 0.1-0.3 mol/L.Investigate with engineering according to the literature, both at home and abroad to the method that the improvement of aluminium casting Waste Sulfuric Acid washing lotion mainly adopts alkali lye to neutralize, precipitate, the shortcoming of this terms of settlement is: not only waste useful sulfuric acid and Tai-Ace S 150 resource, and add neutralizing treatment expense, significantly increase the content of salt in enterprise's waste discharge simultaneously, directly cause the significantly lifting of subsequent wastewater treatment cost.
China Patent No. ZL00228030.2, invention and created name is: a kind of novel aluminum ion is stablized and acid-restoring plant, disclosing one in the specification sheets of this application case utilizes ion exchange resin to block sulfuric acid, thus the method that aluminum ion is separated from waste liquid, the retrieval of sulfuric acid of desorption utilizes.This application case utilizes ion exchange resin to adsorb sulfuric acid, and absorption effluent liquid is aluminum ion solution, and regenerated liquid is sulfuric acid, and because sulfuric acid concentration in Waste Sulfuric Acid is very high, therefore single batch processed amount of this patented method is very limited.
Waste steel slag discharges to obtain waste residue in Steel-making project, and its output accounts for the 15-20% of coarse steel slag output.Current China often produces nearly 200,000,000 tons of steel per year, and slag output about 8,300 ten thousand tons, stores up more than 200,000,000 ton, untreated slag in addition for many years, take up an area nearly 300,000,000 mu.Storing up of slag, not only takies a large amount of arable land, simultaneously contaminate environment, so best outlet is exactly the comprehensive utilization of exploitation slag, turns waste into wealth.
Literature search shows, still does not openly utilize waste steel slag to process the recoverying and utilizing method containing aluminium Waste Sulfuric Acid at present.
Summary of the invention
Object of the present invention is just for above-mentioned the deficiencies in the prior art, provides a kind of recoverying and utilizing method containing aluminium Waste Sulfuric Acid.
The present invention utilizes the waste steel slag process of discharging in steelmaking process containing aluminium Waste Sulfuric Acid, reclaims wherein aluminum oxide and ferric oxide, and consumption acids solution.Its key, in the treatment of wastes with processes of wastes against one another, not only solves the waste of directly discharging pollution to environment and data containing aluminium Waste Sulfuric Acid, has fully utilized the waste steel slag produced in steelmaking process simultaneously, extracted wherein rich in natural resources, reduces environmental pollution.
The technology of the present invention solution is: be achieved through the following technical solutions containing aluminium Waste Sulfuric Acid recoverying and utilizing method:
The waste steel slag of discharging in steelmaking process is joined containing in aluminium Waste Sulfuric Acid, reacting by heating, obtain oxide compound in waste steel slag and containing the acid-respons in aluminium Waste Sulfuric Acid, generate corresponding vitriol and hydrogen, collect hydrogen and provide heat for reacting.Through solid-liquid separation, associating removal of impurities, crystallization, calcining and other processes after reaction terminates, obtain aluminum oxide and ferric oxide.Filter residue after solid-liquid separation is doped in waste steel slag by a certain percentage, makes full use of, and reduces the discharge of solid waste.
The steps include: that (1) raw material prepares: containing aluminium ion concentration in aluminium Waste Sulfuric Acid at 0.1-0.3 mol/L, sulfuric acid concentration is 1-20%; After concentrated by Rotary Evaporators, sulfuric acid concentration is greater than 70%.(2) with liquid-solid ratio be 1-10: 1(containing aluminium Waste Sulfuric Acid and waste steel slag ratio with mL: g for benchmark) waste steel slag is joined containing in aluminium Waste Sulfuric Acid, stir, join in reactor; (3) at temperature of reaction is 50-100 DEG C, 1-3h is reacted; And collect the gas of reaction generation, gas is used for for reaction provides thermal source; (4) reacted solution is carried out filter, associating removal of impurities, crystallization, obtain Tai-Ace S 150 and ferrum sulfuricum oxydatum solutum; There is Tai-Ace S 150 to be known technology with the corresponding oxide that is separated and is converted into of ferric sulfate, be not repeated.Filter the filter residue obtained to be entrained in by a certain percentage in waste steel slag, doping ratio is 1-10: 1(waste steel slag: filter residue) recycle.
Embodiment
Be described in further detail below in conjunction with actual example.
Example one, (1) raw material prepare: containing aluminium ion concentration in aluminium Waste Sulfuric Acid at 0.11 mol/L, sulfuric acid concentration is 5.1%; After concentrated by Rotary Evaporators, sulfuric acid concentration 74.6%; Get above-mentioned containing aluminium Waste Sulfuric Acid 100mL, waste steel slag 10g, waste steel slag is joined containing in aluminium Waste Sulfuric Acid, stirs, join in reactor; (3) at temperature of reaction is 60 DEG C, 1h is reacted; (4) reacted solution is carried out filter, associating removal of impurities, crystallization, obtain Tai-Ace S 150 and ferrum sulfuricum oxydatum solutum; There is Tai-Ace S 150 to be known technology with the corresponding oxide that is separated and is converted into of ferric sulfate, be not repeated.Under this condition, in waste discharge, sulfuric acid concentration drops to less than 0.5%, and the rate of recovery of aluminium reaches 86.0%, and the rate of recovery of iron reaches 84.2%.
Example two, (1) raw material prepare: containing aluminium ion concentration in aluminium Waste Sulfuric Acid at 0.19 mol/L, sulfuric acid concentration is 10.5%; After concentrated by Rotary Evaporators, sulfuric acid concentration 78.3%; (2) get above-mentioned containing aluminium Waste Sulfuric Acid 100mL, waste steel slag 10g, waste steel slag is joined containing in aluminium Waste Sulfuric Acid, stirs, join in reactor; (3) at temperature of reaction is 70 DEG C, 1.5h is reacted; (4) reacted solution is carried out filter, associating removal of impurities, crystallization, obtain Tai-Ace S 150 and ferrum sulfuricum oxydatum solutum; There is Tai-Ace S 150 to be known technology with the corresponding oxide that is separated and is converted into of ferric sulfate, be not repeated.Under this condition, in waste discharge, sulfuric acid concentration drops to less than 0.5%, and the rate of recovery of aluminium reaches 87.3%, and the rate of recovery of iron reaches 84.7%.
Example three, (1) raw material prepare: containing aluminium ion concentration in aluminium Waste Sulfuric Acid at 0.24mol/L, sulfuric acid concentration is 15.3%; After concentrated by Rotary Evaporators, sulfuric acid concentration 79.1%; (2) get above-mentioned containing aluminium Waste Sulfuric Acid 100 mL, waste steel slag 20g, waste steel slag is joined containing in aluminium Waste Sulfuric Acid, stirs, join in reactor; (3) at temperature of reaction is 90 DEG C, 2.5 h are reacted; (4) reacted solution is carried out filter, associating removal of impurities, crystallization, obtain Tai-Ace S 150 and ferrum sulfuricum oxydatum solutum; There is Tai-Ace S 150 to be known technology with the corresponding oxide that is separated and is converted into of ferric sulfate, be not repeated.Under this condition, in waste discharge, sulfuric acid concentration drops to less than 0.5%, and the rate of recovery of aluminium reaches 91.4%, and the rate of recovery of iron reaches 87.8%.
Example four, (1) raw material prepare: containing aluminium ion concentration in aluminium Waste Sulfuric Acid at 0.27 mol/L, sulfuric acid concentration is 6.8%; After concentrated by Rotary Evaporators, sulfuric acid concentration 76.7%; (2) get above-mentioned containing aluminium Waste Sulfuric Acid 100mL, waste steel slag 50g, waste steel slag is joined containing in aluminium Waste Sulfuric Acid, stirs, join in reactor; (3) at temperature of reaction is 70 DEG C, 2h is reacted; (3) reacted solution is carried out filter, associating removal of impurities, crystallization, obtain Tai-Ace S 150 and ferrum sulfuricum oxydatum solutum; There is Tai-Ace S 150 to be known technology with the corresponding oxide that is separated and is converted into of ferric sulfate, be not repeated.Under this condition, in waste discharge, sulfuric acid concentration drops to less than 0.5%, and the rate of recovery of aluminium reaches 89.1%, and the rate of recovery of iron reaches 84.2%.
Example five, (1) raw material prepare: containing aluminium ion concentration in aluminium Waste Sulfuric Acid at 0.13 mol/L, sulfuric acid concentration is 6.7%; After concentrated by Rotary Evaporators, sulfuric acid concentration 70.7%; Be doped in waste steel slag by the filter residue in example three, doping ratio is 5: 1(waste steel slag: filter residue); (2) get above-mentioned containing aluminium Waste Sulfuric Acid 100mL, the mixing slag 50g of waste steel slag and filter residue, joins the mixing slag of waste steel slag and filter residue containing in aluminium Waste Sulfuric Acid, stirs, join in reactor; (3) at temperature of reaction is 60 DEG C, 1h is reacted; (4) reacted solution is carried out filter, associating removal of impurities, crystallization, obtain Tai-Ace S 150 and ferrum sulfuricum oxydatum solutum; There is Tai-Ace S 150 to be known technology with the corresponding oxide that is separated and is converted into of ferric sulfate, be not repeated.Under this condition, in waste discharge, sulfuric acid concentration drops to less than 0.5%, and the rate of recovery of aluminium reaches 84.5%, and the rate of recovery of iron reaches 81.9%.
Example six, (1) raw material prepare: containing aluminium ion concentration in aluminium Waste Sulfuric Acid at 0.13 mol/L, sulfuric acid concentration is 6.7%; After concentrated by Rotary Evaporators, sulfuric acid concentration 79.5%; Be doped in waste steel slag by the filter residue in example three, doping ratio is 1: 1(waste steel slag: filter residue); (2) get above-mentioned containing aluminium Waste Sulfuric Acid 100mL, the mixing slag 50g of waste steel slag and filter residue, joins the mixing slag of waste steel slag and filter residue containing in aluminium Waste Sulfuric Acid, stirs, join in reactor; (3) at temperature of reaction is 60 DEG C, 1h is reacted; (4) reacted solution is carried out filter, associating removal of impurities, crystallization, obtain Tai-Ace S 150 and ferrum sulfuricum oxydatum solutum; There is Tai-Ace S 150 to be known technology with the corresponding oxide that is separated and is converted into of ferric sulfate, be not repeated.Under this condition, in waste discharge, sulfuric acid concentration drops to less than 1%, and the rate of recovery of aluminium reaches 82.4%, and the rate of recovery of iron reaches 80.1%.

Claims (1)

1. containing an aluminium Waste Sulfuric Acid recoverying and utilizing method, it is characterized in that, utilize the waste steel slag process of discharging in steelmaking process containing aluminium Waste Sulfuric Acid, reclaim wherein aluminum oxide and ferric oxide, and consumption acids solution, this recoverying and utilizing method comprises the following steps:
Step one, get a certain amount of containing aluminium Waste Sulfuric Acid in Rotary Evaporators, concentrated containing aluminium Waste Sulfuric Acid; Wherein, containing aluminium ion concentration in aluminium Waste Sulfuric Acid at 0.1-0.3 mol/L, sulfuric acid concentration is 1-20%; Concentrate and be greater than 70% containing sulfuric acid concentration in aluminium Waste Sulfuric Acid;
Step 2, be 1-10: 1 with liquid-solid ratio, with containing aluminium Waste Sulfuric Acid and waste steel slag ratio with mL: g for benchmark, join waste steel slag containing in aluminium Waste Sulfuric Acid, stir, join in reactor, described reactor is with airway and gas extractor;
Material in step 3, step 2 in reactor is 50-100 DEG C in temperature of reaction, and the reaction times is 1-3h; Collecting in reaction process the hydrogen that produces for whole reaction provides thermal source;
Step 4, reacted solution carried out filter, associating removal of impurities, crystallization, obtain Tai-Ace S 150 and ferrum sulfuricum oxydatum solutum; Tai-Ace S 150 is separated with ferric sulfate and is converted into corresponding oxide; Wherein, the filter residue that obtains is filtered in waste steel slag: the ratio of filter residue 1-10: 1 is adulterated recycle again.
CN201310018061.6A 2013-01-18 2013-01-18 A kind of recoverying and utilizing method containing aluminium Waste Sulfuric Acid Expired - Fee Related CN103936041B (en)

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CN106927490B (en) * 2017-04-06 2018-05-15 南通三圣石墨设备科技股份有限公司 Aluminium salt and the method for waste acid recovery are extracted in a kind of acid solution from aluminium containing salt
CN108557855A (en) * 2017-12-20 2018-09-21 大拇指环保设备(天津)有限公司 A kind of resource recycling method of the waste sulfuric acid solution containing aluminium

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1350065A (en) * 2000-10-19 2002-05-22 中国科学院福建物质结构研究所 Comprehensive utilization of waste from aluminium smeltery
CN1672821A (en) * 2005-04-08 2005-09-28 张彭成 Compound treating method of waste industrial sulfuric acid and flyash

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JPS57111215A (en) * 1980-12-29 1982-07-10 Sumitomo Metal Ind Ltd Recovering method of valuable component from metalurgical slag

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1350065A (en) * 2000-10-19 2002-05-22 中国科学院福建物质结构研究所 Comprehensive utilization of waste from aluminium smeltery
CN1672821A (en) * 2005-04-08 2005-09-28 张彭成 Compound treating method of waste industrial sulfuric acid and flyash

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