CN100486908C - Method for preparing aluminium iron polychloride floculant - Google Patents

Method for preparing aluminium iron polychloride floculant Download PDF

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CN100486908C
CN100486908C CNB2006100695044A CN200610069504A CN100486908C CN 100486908 C CN100486908 C CN 100486908C CN B2006100695044 A CNB2006100695044 A CN B2006100695044A CN 200610069504 A CN200610069504 A CN 200610069504A CN 100486908 C CN100486908 C CN 100486908C
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blast furnace
furnace dust
preparation
colloidal sol
aluminium
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CN1935684A (en
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李善评
范思思
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Shandong University
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Shandong University
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Abstract

The invention discloses a polyaluminium iron chloride flocculant preparing method, comprising the steps of: selecting raw materials, preparing blast furnace gas dust solution, preparing Al(OH)3 sol, and preparing polyaluminium iron chloride flocculant; and the prepared product is a compound organic high molecular flocculant and has characters of aluminum and iron salts, and has excellent water purifying performance and wide application range. And it provides a feasible way of synthetically utilizing the wastes of the steel mills and provides a process route with cheap raw materials for flocculant production, achieving the purpose of processing wastes with wastes, and obtaining good economic, social and environmental benefits.

Description

A kind of preparation method of aluminium iron polychloride floculant
Technical field
The present invention relates to the production method of inorganic polymer flocculant, relate in particular to a kind of steel mill waste blast furnace dust that utilizes and prepare the composite type inorganic polymer flocculation agent for main raw material---the method for aluminium iron polychloride.
Background technology
Blast furnace dust is the dust of the crude fuel taken out of with blast furnace gas (also claiming gas) in iron manufacturing process of iron-smelting blast furnace and the particulate that the high-temperature zone intense reaction produces, and its major ingredient is carbon granules, fe and oxide compound thereof, also has SiO in addition 2, Al 2O 3Deng, be one of main solid emission of iron and steel enterprise.The iron and steel output of China leaps to the first in the world in recent years, and the blast furnace dust total amount that iron-smelting blast furnace produces is quite big, and in 1.7% of iron output, nearly 2,000,000 tons of gas ash is produced in the whole nation per year.Because blast furnace dust is the waste residue of ironmaking, quantity is big again, so this must cause adverse influence to environment.
At present, domestic processing mode to blast furnace dust mainly is, each steel mill mostly directly with it as producing cement raw material, clay improvement or producing non-burning brick etc., these defectives of utilizing method are that not only recovery cost is bigger, the program complexity, and economic benefit is low, and environmental protection and energy-saving effect are not remarkable.
The copolymerized type inorganic flocculating agent of ferro-aluminum is the new chemical Industrial products that get up from the seventies to the nineties research and development.Because this flocculation agent has the wide advantage of strong adsorption activity, rapid precipitation and the scope of application of the good flocculation performance and the polymerization iron of polymeric aluminum concurrently, it is had relevant report as a kind of new and effective flocculation agent in American-European and Japan, and obtain certain applying.But, in the report of existing preparation composite inorganic flocculation agent method, be that main raw material prepares aluminium iron polychloride floculant (PAFC) with the blast furnace dust, in the bibliographic data base, have not yet to see the pertinent literature report at home and abroad.
Utilize the blast furnace dust synthetic flocculant, gas ash is utilized effectively, the angle of still creating economic benefit from environment protection all has profound significance.
Summary of the invention
At the deficiencies in the prior art, the object of the present invention is to provide a kind of steel mill waste blast furnace dust that utilizes to prepare the composite type inorganic polymer flocculation agent for main raw material---the method for aluminium iron polychloride.
The preparation method of aluminium iron polychloride floculant of the present invention comprises the steps:
(1) raw material is chosen: with Fe 2O 3Content is no less than 15%, Al 2O 3Content is crossed 60 mesh sieves after being no less than 5% steel mill waste blast furnace dust natural air drying, and is standby;
(2) prepared in laboratory of blast furnace dust dissolution fluid: take by weighing blast furnace dust, put into the four-hole boiling flask that has agitator, thermometer and reflux, add NaF, add mass percent concentration while stirring and be 49% HNO 3With the ferrous iron in the oxidation blast furnace dust, with mass percent concentration 18% hydrochloric acid soln in ash acid than being 1: 1.6～4, temperature of reaction is under 50～105 ℃ of conditions, stirring reaction 1.5～4 hours, make iron, aluminium in the material be dissolved in the liquid phase to greatest extent, suction filtration is mainly contained Al then 3+And Fe 3+The blast furnace dust dissolution fluid, and with ordinary method to its Fe 3+, Al 3+Content detects, and determines iron, aluminium solubility rate;
Above-mentioned blast furnace dust: NaF: mass percent concentration is 49% HNO 3: mass percent concentration is that 18% hydrochloric acid is 50g: 2g: 6ml: 80～200g;
(3) Al (OH) 3The preparation of colloidal sol: get AlCl 36H 2The O crystal is made into Al with deionized water 3+Concentration is about the AlCl of 2.5mol/L 3Solution is 10% Na with mass percent concentration 2CO 3Being neutralized to the pH value is 6.0～6.5, promptly gets Al (OH) 3Colloidal sol;
(4) preparation of aluminium iron polychloride floculant: in the blast furnace dust dissolution fluid that step (2) is produced, add the Al (OH) that step (3) is produced gradually 3Colloidal sol, the colloidal sol add-on is with dissolution fluid and generation Al (OH) 3The AlCl of colloidal sol 3The volume ratio of solution counts 1: 1～and 2, be under 20～70 ℃ of conditions in the hydrolytic polymerization temperature, stirring reaction 2～4 hours, static slaking 24 ± 2 hours promptly gets reddish-brown aluminium iron polychloride liquid flocculation agent.
Among the preparation method of above-mentioned aluminium iron polychloride floculant: the described ash acid of step (2) than be preferably 1: 2.5～3.5, temperature of reaction is preferably 80～100 ℃, the stirring reaction time is preferably 2.5～3.5 hours.
Wherein: the described ash acid of step (2) is than most preferably being 1: 3, and temperature of reaction most preferably is 100 ℃, and the stirring reaction time optimal is elected 3 hours as.
Among the preparation method of above-mentioned aluminium iron polychloride floculant: the described colloidal sol add-on of step (4) is with dissolution fluid and generation Al (OH) 3The AlCl of colloidal sol 3The volume ratio meter of solution is preferably 1: 1.
Among the preparation method of above-mentioned aluminium iron polychloride floculant: the described hydrolytic polymerization temperature of step (4) is preferably 50～70 ℃, and the stirring reaction time is preferably 3～4 hours.
Wherein: the described hydrolytic polymerization temperature of step (4) most preferably is 60～70 ℃, and the stirring reaction time optimal is elected 4 hours as.
The preparation method of aluminium iron polychloride floculant of the present invention have process innovation, method easy, with low cost, be beneficial to outstanding advantages such as ring protection, the product appearance of producing is a reddish-brown liquid, density is 1.2g/mL, pH value 3.5, basicity 57.0%, Al 2O 3The quality percentage composition is 10.8%, Fe 2O 3The quality percentage composition is 3.6%.Product has good flocculating property and broad field of application, economic benefit, social benefit, obvious environment benefit.
The advantage that the present invention is compared with prior art possessed is:
(1) utilizes steel mill waste to be raw material, can reduce the production cost and the cost for wastewater treatment of aluminium iron polychloride greatly, help applying of this novel flocculant;
The removal of COD when (2) the high meeting of ferrous content influence water treatment in the poly-ferro-aluminum flocculation agent, present method is a catalyzer owing to having adopted strong oxidizer nitric acid, does not almost have Fe in the PAFC product 2+, flocculating effect is remarkable, handles malting effluent, its COD with this flocculation agent CrClearance reaches about 45%, and the SS clearance reaches more than 90%;
(3) steel mill's solid waste is fully utilized, when reducing the inorganic polymer flocculant production cost, can improve its environmental value again, reach the purpose of the treatment of wastes with processes of wastes against one another, realize the resource utilization of solid waste, for a new way is explored in the recycling of steel mill waste blast furnace dust;
(4) product is stable, and low-consuming, the pH value scope of application is wide, and settling property is good;
(5) need not pressurize in the building-up process, oxygenation, simple to operate, reduced investment, instant effect has tangible practical value.
Description of drawings
Fig. 1 is a synthesis process flow diagram of the present invention.
Embodiment
The present invention is described in detail below in conjunction with accompanying drawing.
Embodiment 1
As shown in Figure 1, utilizing the steel mill waste blast furnace dust to prepare composite type inorganic polymer flocculant poly aluminium chloride ferrum liquid product may further comprise the steps:
(1) raw material is chosen: with Fe 2O 3Content is 24.32%, Al 2O 3Content is to cross 60 mesh sieves behind 8.42% the steel mill waste blast furnace dust natural air drying, and is standby;
(2) prepared in laboratory of blast furnace dust dissolution fluid: take by weighing the 50g blast furnace dust, put into the 500mL four-hole boiling flask that has agitator, thermometer and reflux, add 2gNaF, add the 6mL mass percent concentration while stirring and be 49% HNO 3With the ferrous iron in the oxidation blast furnace dust, with mass percent concentration be 18% hydrochloric acid soln in ash acid than being 1: 3, temperature of reaction is under 100～105 ℃ of conditions, stirring reaction 3 hours, iron, aluminium in the material are dissolved in the liquid phase to greatest extent, and suction filtration is mainly contained Al then 3+And Fe 3+The blast furnace dust dissolution fluid, and with ordinary method to its Fe 3+, Al 3+Content detects, and records its iron, the aluminium solubility rate is respectively 67.61% and 12.35%;
(3) Al (OH) 3The preparation of colloidal sol: get AlCl 36H 2The O crystal is made into Al with deionized water 3+Concentration is about the AlCl of 2.5mol/L 3Solution is 10% Na with mass percent concentration 2CO 3Being neutralized to the pH value is 6.0～6.5, promptly gets Al (OH) 3Colloidal sol;
(4) preparation of aluminium iron polychloride floculant: in the blast furnace dust dissolution fluid that step (2) is produced, add the Al (OH) that step (3) is produced gradually 3Colloidal sol, the colloidal sol add-on is with dissolution fluid and generation Al (OH) 3The AlCl of colloidal sol 3The volume ratio of solution is counted 1: 1, is under 60～70 ℃ of conditions in the hydrolytic polymerization temperature, stirring reaction 4 hours, and static slaking 24 hours promptly gets reddish-brown aluminium iron polychloride liquid flocculation agent.
Embodiment 2
Utilize the steel mill waste blast furnace dust to prepare the method for aluminium iron polychloride liquid flocculation agent, may further comprise the steps:
(1) raw material is chosen: with Fe 2O 3Content is 21.2%, Al 2O 3Content is to cross 60 mesh sieves behind 7.8% the steel mill waste blast furnace dust natural air drying, and is standby;
(2) prepared in laboratory of blast furnace dust dissolution fluid: take by weighing the 50g blast furnace dust, put into the 500mL four-hole boiling flask that has agitator, thermometer and reflux, add 2gNaF, add the 6mL mass percent concentration while stirring and be 49% HNO 3With the ferrous iron in the oxidation blast furnace dust, with mass percent concentration be 18% hydrochloric acid soln in ash acid than being 1: 4, temperature of reaction is under 70～85 ℃ of conditions, stirring reaction 2 hours, iron, aluminium in the material are dissolved in the liquid phase to greatest extent, and suction filtration is mainly contained Al then 3+And Fe 3+The blast furnace dust dissolution fluid, and with ordinary method to its Fe 3+, Al 3+Content detects, and records its iron, the aluminium solubility rate is respectively 59.4% and 10.5%;
(3) Al (OH) 3The preparation of colloidal sol: get AlCl 36H 2The O crystal is made into Al with deionized water 3+Concentration is about the AlCl of 2.5mol/L 3Solution is 10% Na with mass percent concentration 2CO 3Being neutralized to the pH value is 6.2～6.5, promptly gets Al (OH) 3Colloidal sol;
(4) preparation of aluminium iron polychloride floculant: in the blast furnace dust dissolution fluid that step (2) is produced, add the Al (OH) that step (3) is produced gradually 3Colloidal sol, the colloidal sol add-on is with dissolution fluid and generation Al (OH) 3The AlCl of colloidal sol 3The volume ratio of solution is counted 1: 1.5, is under 45～50 ℃ of conditions in the hydrolytic polymerization temperature, stirring reaction 3 hours, and static slaking 26 hours promptly gets reddish-brown aluminium iron polychloride liquid flocculation agent.
Embodiment 3
Utilize the steel mill waste blast furnace dust to prepare the method for aluminium iron polychloride liquid flocculation agent, may further comprise the steps:
(1) raw material is chosen: with Fe 2O 3Content is 25.2%, Al 2O 3Content is to cross 60 mesh sieves behind 8.8% the steel mill waste blast furnace dust natural air drying, and is standby;
(2) prepared in laboratory of blast furnace dust dissolution fluid: take by weighing the 50g blast furnace dust, put into the 500mL four-hole boiling flask that has agitator, thermometer and reflux, add 2gNaF, add the 6mL mass percent concentration while stirring and be 49% HNO 3With the ferrous iron in the oxidation blast furnace dust, with mass percent concentration be 18% hydrochloric acid soln in ash acid than being 1: 2, temperature of reaction is under 50～65 ℃ of conditions, stirring reaction 4 hours, iron, aluminium in the material are dissolved in the liquid phase to greatest extent, and suction filtration is mainly contained Al then 3+And Fe 3+The blast furnace dust dissolution fluid, and with ordinary method to its Fe 3+, Al 3+Content detects, and records its iron, the aluminium solubility rate is respectively 69.4% and 13.2%;
(3) Al (OH) 3The preparation of colloidal sol: get AlCl 36H 2The O crystal is made into Al with deionized water 3+Concentration is about the AlCl of 2.5mol/L 3Solution is 10% Na with mass percent concentration 2CO 3Being neutralized to the pH value is 6.2～6.3, promptly gets Al (OH) 3Colloidal sol;
(4) preparation of aluminium iron polychloride floculant: in the blast furnace dust dissolution fluid that step (2) is produced, add the Al (OH) that step (3) is produced gradually 3Colloidal sol, the colloidal sol add-on is with dissolution fluid and generation Al (OH) 3The AlCl of colloidal sol 3The volume ratio of solution is counted 1: 1.2, is under 25～35 ℃ of conditions in the hydrolytic polymerization temperature, stirring reaction 4 hours, and static slaking 25 hours promptly gets reddish-brown aluminium iron polychloride liquid flocculation agent.

Claims (6)

1. the preparation method of an aluminium iron polychloride floculant comprises the steps:
(1) raw material is chosen: with Fe 2O 3Content is no less than 15%, Al 2O 3Content is crossed 60 mesh sieves after being no less than 5% steel mill waste blast furnace dust natural air drying, and is standby;
(2) prepared in laboratory of blast furnace dust dissolution fluid: take by weighing blast furnace dust, put into the four-hole boiling flask that has agitator, thermometer and reflux, add NaF, add mass percent concentration while stirring and be 49% HNO 3With the ferrous iron in the oxidation blast furnace dust, with mass percent concentration 18% hydrochloric acid soln in ash acid than being 1: 1.6～4, temperature of reaction is under 50～105 ℃ of conditions, stirring reaction 1.5～4 hours, make iron, aluminium in the material be dissolved in the liquid phase to greatest extent, suction filtration is mainly contained Al then 3+And Fe 3+The blast furnace dust dissolution fluid, and with ordinary method to its Fe 3+, Al 3+Content detects, and determines iron, aluminium solubility rate;
Above-mentioned blast furnace dust: NaF: mass percent concentration is 49% HNO 3: mass percent concentration is that 18% hydrochloric acid is 50g: 2g: 6ml: 80～200g;
(3) Al (OH) 3The preparation of colloidal sol: get AlCl 36H 2The O crystal is made into Al with deionized water 3+Concentration is about the AlCl of 2.5mol/L 3Solution is 10% Na with mass percent concentration 2CO 3Being neutralized to the pH value is 6.0～6.5, promptly gets Al (OH) 3Colloidal sol;
(4) preparation of aluminium iron polychloride floculant: in the blast furnace dust dissolution fluid that step (2) is produced, add the Al (OH) that step (3) is produced gradually 3Colloidal sol, the colloidal sol add-on is with dissolution fluid and generation Al (OH) 3The AlCl of colloidal sol 3The volume ratio of solution counts 1: 1～and 2, be under 20～70 ℃ of conditions in the hydrolytic polymerization temperature, stirring reaction 2～4 hours, static slaking 24 ± 2 hours promptly gets reddish-brown aluminium iron polychloride liquid flocculation agent.
2. the preparation method of aluminium iron polychloride floculant as claimed in claim 1 is characterized in that: the described ash acid of step (2) is than being 1: 2.5～3.5, and temperature of reaction is 80～100 ℃, and the stirring reaction time is 2.5～3.5 hours.
3. the preparation method of aluminium iron polychloride floculant as claimed in claim 2 is characterized in that: the described ash acid of step (2) is than being 1: 3, and temperature of reaction is 100 ℃, and the stirring reaction time is 3 hours.
4. the preparation method of aluminium iron polychloride floculant as claimed in claim 1 is characterized in that: the described colloidal sol add-on of step (4) with dissolution fluid with generate Al (OH) 3The AlCl of colloidal sol 3The volume ratio of solution is counted 1: 1.
5. the preparation method of aluminium iron polychloride floculant as claimed in claim 1, it is characterized in that: the described hydrolytic polymerization temperature of step (4) is 50～70 ℃, and the stirring reaction time is 3～4 hours.
6. the preparation method of aluminium iron polychloride floculant as claimed in claim 5, it is characterized in that: the described hydrolytic polymerization temperature of step (4) is 60～70 ℃, and the stirring reaction time is 4 hours.
CNB2006100695044A 2006-10-20 2006-10-20 Method for preparing aluminium iron polychloride floculant Expired - Fee Related CN100486908C (en)

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Publication number Priority date Publication date Assignee Title
CN101575130B (en) * 2009-06-15 2011-01-05 山东大学 Method for preparing rare earth ceria modified inorganic polymeric flocculant by using industrial waste
CN107055625A (en) * 2017-05-31 2017-08-18 江苏省冶金设计院有限公司 The apparatus and method that a kind of utilization magnetic separation tailings prepares PAFC
CN107055626A (en) * 2017-05-31 2017-08-18 江苏省冶金设计院有限公司 A kind of method and apparatus for preparing PAFC using hot metallurgical slag

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