CN103936041A - Method for recovering and utilizing aluminum-containing waste sulfuric acid - Google Patents
Method for recovering and utilizing aluminum-containing waste sulfuric acid Download PDFInfo
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- CN103936041A CN103936041A CN201310018061.6A CN201310018061A CN103936041A CN 103936041 A CN103936041 A CN 103936041A CN 201310018061 A CN201310018061 A CN 201310018061A CN 103936041 A CN103936041 A CN 103936041A
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Abstract
The invention discloses a method for recovering and utilizing aluminum-containing waste sulfuric acid, and belongs to the technical field of joint recovery and utilization of aluminum-containing waste acids and solid wastes. The method utilizes the waste iron slag discharged during the steel making process to react with aluminum-containing waste sulfuric acid to reduce the sulfuric acid content in the waste acid, wherein the sulfuric acid content can be reduced to 1% or less, and aluminum oxide and iron oxide in the waste acid are recovered at the same time. The method comprises the following steps: utilizing a rotary evaporator to process aluminum-containing waste sulfuric acid until the sulfuric acid content exceeds 70%; adding waste steel slag into the condensed aluminum-containing waste sulfuric acid according to a certain solid/liquid ratio, wherein the aluminum-containing waste sulfuric acid is measured by volume (mL), and the waste steel slag is measured by weight (g); controlling the operation temperature in a range of 50 to 100 DEG C, and the reaction time in a range of 1 to 3 hours; recovering the hydrogen gas generated during the reaction process, burning the hydrogen gas to provide a heat source for the reactions; and then subjecting the reaction product to processes of solid/liquid separation, joint impurity removing, crystallization, and burning so as to obtain aluminum oxide solid and iron oxide solid; wherein the filter slag generated in the solid/liquid separation process can be mixed with the waste steel slag according to a ratio of waste steel slag to filter slag of (1-10): 1, and thus circulation utilization is achieved. The method utilizes the waste steel slag generated during the steel making process to process waste aluminum-containing waste sulfuric acid, processes wastes by using wastes, and achieves the joint treatment and resource recovery of liquid wastes and solid wastes.
Description
(1) technical field
The invention belongs to a kind of recoverying and utilizing method containing aluminium Waste Sulfuric Acid, particularly utilize technical field containing the combined recovery of aluminium Waste Sulfuric Acid and solid waste.
(2) background technology
The industries such as automobile, household electrical appliances, aviation, mechanical means, plating, metallurgy are used aluminium and aluminum alloy casting as starting material in a large number.These aluminium castings use and go to toward utilizing the vitriol oil to flood and rinsing.The sulfuric acid concentration of this Waste Sulfuric Acid washing lotion is 1-20%, and aluminium composition is 0.1-0.3mol/L.Investigate with engineering according to the literature, the improvement of aluminium casting Waste Sulfuric Acid washing lotion is mainly adopted the method for alkali lye neutralization, precipitation both at home and abroad, the shortcoming of this terms of settlement is: not only wasted useful sulfuric acid and Tai-Ace S 150 resource, and increase neutralizing treatment expense, the content that has significantly increased salt in enterprise's waste discharge, directly causes the significantly lifting of subsequent wastewater treatment cost simultaneously.
China Patent No. ZL00228030.2, invention and created name is: a kind of novel aluminum ion is stablized and acid-restoring plant, in the specification sheets of this application case, disclose one and utilized ion exchange resin retardance sulfuric acid, thus the method that aluminum ion is separated from waste liquid, the retrieval of sulfuric acid utilization of desorption.This application case is to utilize ion exchange resin absorption 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 is in Steel-making project, to discharge to obtain waste residue, and its output accounts for the 15-20% of coarse steel slag output.Nearly 200,000,000 tons of the every annual output steel of China at present, approximately 8,300 ten thousand tons of slag output are stored 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 lands, and contaminate environment simultaneously, so best outlet is exactly the comprehensive utilization of exploitation slag, turns waste into wealth.
Literature search shows, does not still openly utilize waste steel slag to process the recoverying and utilizing method containing aluminium Waste Sulfuric Acid at present.
(3) summary of the invention
Object of the present invention is just for above-mentioned the deficiencies in the prior art, and a kind of recoverying and utilizing method containing aluminium Waste Sulfuric Acid is provided.
The present invention utilizes the waste steel slag of discharging in steelmaking process to process containing aluminium Waste Sulfuric Acid, reclaims wherein aluminum oxide and ferric oxide, and consumption acids solution.Its key is in the treatment of wastes with processes of wastes against one another, not only solves containing aluminium Waste Sulfuric Acid and directly discharges pollution to environment and the waste of data, fully utilized the waste steel slag producing in steelmaking process simultaneously, extracts wherein rich in natural resources, minimizing 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, and reacting by heating, obtains oxide compound and containing the acid-respons in aluminium Waste Sulfuric Acid, generates corresponding vitriol and hydrogen in waste steel slag, collect hydrogen and provide heat for reacting.After finishing, reaction through solid-liquid separation, associating removal of impurities, crystallization, calcining and other processes, obtains 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:
(1) raw material is prepared: containing aluminium ion concentration in aluminium Waste Sulfuric Acid, at 0.1-0.3mol/L, sulfuric acid concentration is 1-20%; After concentrating by Rotary Evaporators, sulfuric acid concentration is greater than 70%.
(2) taking liquid-solid ratio as 1-10: join waste steel slag containing in aluminium Waste Sulfuric Acid for 1 (containing aluminium Waste Sulfuric Acid and waste steel slag ratio taking mL: g as benchmark), stirs, and joins in reactor;
(3) be to react 1-3h at 50-100 DEG C in temperature of reaction; And collect the gas that reaction produces, gas is used to reaction that thermal source is provided;
(4) reacted solution is filtered, associating removal of impurities, crystallization, obtain Tai-Ace S 150 and ferrum sulfuricum oxydatum solutum; Having the corresponding oxide that separates and be converted into of Tai-Ace S 150 and ferric sulfate is known technology, is not repeated.
The filter residue that filtration obtains is entrained in waste steel slag by a certain percentage, and doping ratio is 1-10: 1 (waste steel slag: filter residue) recycle.
(4) embodiment
Be described in further detail below in conjunction with actual example:
Example one
(1) raw material is prepared: containing aluminium ion concentration in aluminium Waste Sulfuric Acid, at 0.11mol/L, sulfuric acid concentration is 5.1%; After concentrating by Rotary Evaporators, sulfuric acid concentration 74.6%;
(2) get the above-mentioned aluminium Waste Sulfuric Acid 100mL of containing, waste steel slag 10g, joins waste steel slag containing in aluminium Waste Sulfuric Acid, stirs, and joins in reactor;
(3) be to react 1h at 60 DEG C in temperature of reaction;
(4) reacted solution is filtered, associating removal of impurities, crystallization, obtain Tai-Ace S 150 and ferrum sulfuricum oxydatum solutum; Having the corresponding oxide that separates and be converted into of Tai-Ace S 150 and ferric sulfate is known technology, is not repeated.
Under this condition, in waste discharge, sulfuric acid concentration drops to below 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 is prepared: containing aluminium ion concentration in aluminium Waste Sulfuric Acid, at 0.19mol/L, sulfuric acid concentration is 10.5%; After concentrating by Rotary Evaporators, sulfuric acid concentration 78.3%;
(2) get the above-mentioned aluminium Waste Sulfuric Acid 100mL of containing, waste steel slag 10g, joins waste steel slag containing in aluminium Waste Sulfuric Acid, stirs, and joins in reactor;
(3) be to react 1.5h at 70 DEG C in temperature of reaction;
(4) reacted solution is filtered, associating removal of impurities, crystallization, obtain Tai-Ace S 150 and ferrum sulfuricum oxydatum solutum; Having the corresponding oxide that separates and be converted into of Tai-Ace S 150 and ferric sulfate is known technology, is not repeated.
Under this condition, in waste discharge, sulfuric acid concentration drops to below 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 is prepared: containing aluminium ion concentration in aluminium Waste Sulfuric Acid, at 0.24mol/L, sulfuric acid concentration is 15.3%; After concentrating by Rotary Evaporators, sulfuric acid concentration 79.1%;
(2) get the above-mentioned aluminium Waste Sulfuric Acid 100mL of containing, waste steel slag 20g, joins waste steel slag containing in aluminium Waste Sulfuric Acid, stirs, and joins in reactor;
(3) be to react 2.5h at 90 DEG C in temperature of reaction;
(4) reacted solution is filtered, associating removal of impurities, crystallization, obtain Tai-Ace S 150 and ferrum sulfuricum oxydatum solutum; Having the corresponding oxide that separates and be converted into of Tai-Ace S 150 and ferric sulfate is known technology, is not repeated.
Under this condition, in waste discharge, sulfuric acid concentration drops to below 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 is prepared: containing aluminium ion concentration in aluminium Waste Sulfuric Acid, at 0.27mol/L, sulfuric acid concentration is 6.8%; After concentrating by Rotary Evaporators, sulfuric acid concentration 76.7%;
(2) get the above-mentioned aluminium Waste Sulfuric Acid 100mL of containing, waste steel slag 50g, joins waste steel slag containing in aluminium Waste Sulfuric Acid, stirs, and joins in reactor;
(3) be to react 2h at 70 DEG C in temperature of reaction;
(4) reacted solution is filtered, associating removal of impurities, crystallization, obtain Tai-Ace S 150 and ferrum sulfuricum oxydatum solutum; Having the corresponding oxide that separates and be converted into of Tai-Ace S 150 and ferric sulfate is known technology, is not repeated.
Under this condition, in waste discharge, sulfuric acid concentration drops to below 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 is prepared: containing aluminium ion concentration in aluminium Waste Sulfuric Acid, at 0.13mol/L, sulfuric acid concentration is 6.7%; After concentrating by Rotary Evaporators, sulfuric acid concentration 70.7%; Filter residue in example three is doped in waste steel slag, and doping ratio is 5: 1 (waste steel slag: filter residue);
(2) get the above-mentioned aluminium Waste Sulfuric Acid 100mL of containing, 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, and joins in reactor;
(3) be to react 1h at 60 DEG C in temperature of reaction;
(4) reacted solution is filtered, associating removal of impurities, crystallization, obtain Tai-Ace S 150 and ferrum sulfuricum oxydatum solutum; Having the corresponding oxide that separates and be converted into of Tai-Ace S 150 and ferric sulfate is known technology, is not repeated.
Under this condition, in waste discharge, sulfuric acid concentration drops to below 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 is prepared: containing aluminium ion concentration in aluminium Waste Sulfuric Acid, at 0.13mol/L, sulfuric acid concentration is 6.7%; After concentrating by Rotary Evaporators, sulfuric acid concentration 79.5%; Filter residue in example three is doped in waste steel slag, and doping ratio is 1: 1 (waste steel slag: filter residue);
(2) get the above-mentioned aluminium Waste Sulfuric Acid 100mL of containing, 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, and joins in reactor;
(3) be to react 1h at 60 DEG C in temperature of reaction;
(4) reacted solution is filtered, associating removal of impurities, crystallization, obtain Tai-Ace S 150 and ferrum sulfuricum oxydatum solutum; Having the corresponding oxide that separates and be converted into of Tai-Ace S 150 and ferric sulfate is known technology, is not repeated.
Under this condition, in waste discharge, sulfuric acid concentration drops to below 1%, and the rate of recovery of aluminium reaches 82.4%, and the rate of recovery of iron reaches 80.1%.
Claims (9)
1. containing an aluminium Waste Sulfuric Acid recoverying and utilizing method, it is characterized in that, utilize the waste steel slag of discharging in steelmaking process to process containing aluminium Waste Sulfuric Acid, reclaim wherein aluminum oxide and ferric oxide, and consumption acids solution.
2. it is characterized in that containing aluminium Waste Sulfuric Acid recoverying and utilizing method according to claimed in claim 1, comprise following order and step:
Step 1, get a certain amount of containing aluminium Waste Sulfuric Acid in Rotary Evaporators, concentrated containing aluminium Waste Sulfuric Acid;
Step 2, taking liquid-solid ratio as 1-10: 1 (containing aluminium Waste Sulfuric Acid and waste steel slag ratio taking mL: g as benchmark) joins waste steel slag containing in aluminium Waste Sulfuric Acid, stirs, and joins in reactor;
Step 3, react for some time at a certain temperature;
Step 4, by reacted solution filter, associating removal of impurities, crystallization, obtain Tai-Ace S 150 and ferrum sulfuricum oxydatum solutum; Having the corresponding oxide that separates and be converted into of Tai-Ace S 150 and ferric sulfate is known technology, is not repeated.
3. according to claim 2 containing aluminium Waste Sulfuric Acid recoverying and utilizing method, its feature in step 1 containing aluminium ion concentration in aluminium Waste Sulfuric Acid at 0.1-0.3mol/L, sulfuric acid concentration is 1-20%.
4. according to claim 2 containing aluminium Waste Sulfuric Acid recoverying and utilizing method, its feature concentrates containing sulfuric acid concentration in aluminium Waste Sulfuric Acid and is greater than 70% in step 1.
5. according to claim 2 containing aluminium Waste Sulfuric Acid recoverying and utilizing method, its feature in step 2 reactor with airway and gas extractor.
6. according to claim 2 containing aluminium Waste Sulfuric Acid recoverying and utilizing method, its feature temperature of reaction in step 2 is 50-100 DEG C, and the reaction times is 1-3h.
7. according to claim 2 containing aluminium Waste Sulfuric Acid recoverying and utilizing method, its feature is filtered the filter residue obtaining and is entrained in by a certain percentage in waste steel slag in step 3, recycle.
8. according to claim 3 containing aluminium Waste Sulfuric Acid recoverying and utilizing method, it is characterized in that, the hydrogen of collection is used to the reaction in claim 2 that thermal source is provided.
9. according to claim 7 containing aluminium Waste Sulfuric Acid recoverying and utilizing method, it is characterized in that, the ratio of its doping is 1-10: 1 (waste steel slag: filter residue).
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| CN201310018061.6A CN103936041B (en) | 2013-01-18 | 2013-01-18 | A kind of recoverying and utilizing method containing aluminium Waste Sulfuric Acid |
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| CN201310018061.6A CN103936041B (en) | 2013-01-18 | 2013-01-18 | A kind of recoverying and utilizing method containing aluminium Waste Sulfuric Acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106927490A (en) * | 2017-04-06 | 2017-07-07 | 南通三圣石墨设备科技股份有限公司 | A kind of method that aluminium salt and waste acid recovery are extracted in 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 (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57111215A (en) * | 1980-12-29 | 1982-07-10 | Sumitomo Metal Ind Ltd | Recovering method of valuable component from metalurgical slag |
| 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 |
-
2013
- 2013-01-18 CN CN201310018061.6A patent/CN103936041B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57111215A (en) * | 1980-12-29 | 1982-07-10 | Sumitomo Metal Ind Ltd | Recovering method of valuable component from metalurgical slag |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106927490A (en) * | 2017-04-06 | 2017-07-07 | 南通三圣石墨设备科技股份有限公司 | A kind of method that aluminium salt and waste acid recovery are extracted in acid solution from aluminium containing salt |
| 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 |
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| CN103936041B (en) | 2015-10-14 |
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