CN105502516B - A kind of method that poly-iron chloride is prepared by iron and steel pickling waste liquid - Google Patents
A kind of method that poly-iron chloride is prepared by iron and steel pickling waste liquid Download PDFInfo
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- CN105502516B CN105502516B CN201610084067.7A CN201610084067A CN105502516B CN 105502516 B CN105502516 B CN 105502516B CN 201610084067 A CN201610084067 A CN 201610084067A CN 105502516 B CN105502516 B CN 105502516B
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- C01—INORGANIC CHEMISTRY
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- C01G49/00—Compounds of iron
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Abstract
The invention discloses a kind of method that poly-iron chloride is prepared by iron and steel pickling waste liquid, step is：(1) iron and steel pickling waste liquid is taken, reducing agent is added, stirring is placed；(2) double purification treatment；(3) hydrochloric acid, the aqueous solution of stabilizer is added under stirring, to be passed through air oxidation；(4) molar content of solution ferrous ions is regularly determined in air event is passed through, when solution ferrous ions account for 5% the 40% of the total molar content of iron, stopping is passed through air, oxidant is added to continue to aoxidize remaining ferrous ion, untill in solution without ferrous ion, the transparent poly-iron chloride liquid of yellowish-brown is obtained.Of the invention thoroughly to solve pollution of the pickle liquor to environment, realizing turns waste into wealth；Invest that low, low cost, efficiency high, technological operation be simple, production safety is environmentally friendly, products obtained therefrom is that outward appearance is yellowish-brown transparency liquid, can be with stable existence more than six months, flocculating effect is good, is widely used in sewage disposal.
Description
Technical field
It is more particularly to a kind of to be prepared by iron and steel pickling waste liquid the present invention relates to inorganic polymer functional material preparation field
The method of poly-iron chloride.
Background technology
It is well known that pickling is essential process for treating surface during pickling iron and steel, the side of technology chemistry
Method removes the oxide layer of steel surface.Contain substantial amounts of ferrous salt and residual acid in acid pickle after pickling, if untreated
Just directly discharge, iron and steel pickling waste liquid will cause huge harm to environment.To the treatment technology of pickling iron and steel acid pickle in text
In offering it has been reported that but these processing methods operation condition it is harsh, complex process, high cost is difficult to realize industrialization.Cause
This, find a kind of effective method recycle pickling iron and steel acid pickle be allowed to be converted into useful product be we face one
The urgent task of item.Poly-ferric chloride is a kind of new and effective inorganic polymer coagulation water purification agent, i.e. water treatment agent, is industry
With required chemical agent in water, domestic water, wastewater treatment process.Water purification agent is mainly used to control the shape of incrustation scale and sludge
Into, reduce foam, reduction contacted with water material corrosion, removing water in suspended solid and noxious material, deodorization and discoloration, softening
Water quality etc..By using poly-ferric chloride, water can be made to reach certain quality requirement.With in world wide to Global Ecological ring
The need for border, the attention of sustainable development and the development of new and high technology, acquisition raw material prepares polyaluminium from secondary resource
Silicic acid is one one of recycling treatment pickling iron and steel acid pickle selection well.
The content of the invention
The problem of the technology faced present invention aim to address current domestic steel industry treatment iron and steel pickling waste liquid,
A kind of method that poly-iron chloride is prepared by iron and steel pickling waste liquid is provided.
Technical scheme is summarized as follows：
A kind of method that poly-iron chloride is prepared by iron and steel pickling waste liquid, comprises the following steps：
(1) pretreatment of iron and steel pickling waste liquid：Iron and steel pickling waste liquid is taken, reducing agent reduction ferric iron is added, makes reducing agent
Mass content is 0.2%~1%, is stirred, and places 2-10h；
(2) double purification treatment：Under agitation, pH=4~8 of pretreated iron and steel pickling waste liquid are adjusted with alkali, plus
Entering auxiliary agent makes final concentration of 45~70mg/l, at 40~80 DEG C, reacts 0.5-3h, stands, filters, after obtaining double purification treatment
Solution, surveys Fe in solutionAlwaysMass concentration；
(3) HCl and Fe is made to addition hydrochloric acid in the solution of step (2) acquisitionAlwaysMass ratio be 0.45-0.55, add steady
Determine the aqueous solution of agent, make stabilizer and FeAlwaysMol ratio=0.12-0.30, at 15-70 DEG C, under 100-400rpm stirrings, to flow
It is 0.05~0.2m to measure3/ h is passed through air oxidation；
(4) molar content of solution ferrous ions is regularly determined in air event is passed through, when solution ferrous ions
When accounting for the 5%-40% of the total molar content of iron, stopping is passed through air, adds oxidant to continue to aoxidize remaining ferrous ion, until
Without untill ferrous ion in solution, the transparent poly-iron chloride liquid of yellowish-brown is obtained.
Step (1) the reducing agent mass content is preferably 0.5%~1%.
The reducing agent is preferably iron filings or scrap iron skin.
The treatment of step (2) double purification is preferably：Under agitation, the pH of pretreated iron and steel pickling waste liquid is adjusted with alkali
=5~7, add auxiliary agent to make final concentration of 50~65mg/l, at 50~65 DEG C, 0.5-3h is stirred, filtering obtains molten after after-treatment
Liquid, surveys Fe in solutionAlwaysMass concentration.
Alkali is preferably NaOH, ammoniacal liquor, sodium carbonate or sodium acid carbonate.
Auxiliary agent is preferably polyacrylamide.
Stabilizer is preferably in acetic acid, citric acid, phosphoric acid, phosphate, dibasic alkaliine, dihydric phosphate and silicic acid
Plant or two kinds.
Oxidant is preferably H2O2Or NaClO3。
Recycling treatment is carried out to iron and steel pickling waste liquid with the method for the present invention, there is no any produce in whole preparation process
It is raw, thoroughly solve pollution of the pickle liquor to environment；Being realized with the inventive method turns waste into wealth；The method of the present invention is invested
Low, low cost, efficiency high, technological operation are simple, production safety is environmentally friendly, and products obtained therefrom is the transparent polychloride iron liquid of yellowish-brown
Body, can be with stable existence more than six months, and flocculating effect is good, is widely used in sewage disposal, is steel industry treatment pickling
Waste liquid provides a kind of good technical scheme.
Specific embodiment
With reference to specific embodiment, the present invention is further illustrated, and the following examples are in order that this area
Technical staff better understood when the present invention, but the present invention not imposed any restrictions.
Embodiment 1
A kind of method that poly-iron chloride is prepared by iron and steel pickling waste liquid, comprises the following steps：
(1) pretreatment of iron and steel pickling waste liquid：Iron and steel pickling waste liquid is taken, iron reduction ferric iron is added, makes iron filings quality
Content is 0.2%, is stirred, and places 10h；
(2) double purification treatment：Under agitation, the pH=7 of pretreated iron and steel pickling waste liquid is adjusted with ammoniacal liquor, is added
Polyacrylamide makes final concentration of 50mg/l, at 65 DEG C, reacts 0.5h, stands, filters, and obtains the solution after double purification treatment,
Survey Fe in solutionAlwaysMass concentration；
(3) the middle addition 17ml concentrated hydrochloric acids of solution (mass concentration is 151.2g/L) obtained to 100ml steps (2) make HCl
And FeAlwaysMass ratio be 0.55, add stabilizer the aqueous solution (stabilizer is 5.65g sodium phosphates), make stabilizer and FeAlwaysRub
That ratio=0.12, at 70 DEG C, under 400rpm stirrings, with flow as 0.05m3/ h is passed through air oxidation；
(4) molar content of solution ferrous ions is regularly determined in air event is passed through, when solution ferrous ions
When accounting for the 5% of the total molar content of iron, stopping is passed through air, adds 5.7g NaClO3Continue to aoxidize remaining ferrous ion, until
Without untill ferrous ion in solution, the transparent poly-iron chloride liquid of 122.65ml yellowish-brown is obtained.Product can be with stable existence 8
Individual month.
Embodiment 2
A kind of method that poly-iron chloride is prepared by iron and steel pickling waste liquid, comprises the following steps：
(1) pretreatment of iron and steel pickling waste liquid：Iron and steel pickling waste liquid is taken, scrap iron skin reduction ferric iron is added, makes scrap iron skin
Mass content is 0.5%, is stirred, and places 5h；
(2) double purification treatment：Under agitation, pretreated iron and steel pickling waste liquid is adjusted with sodium hydrate aqueous solution
PH=5, adds polyacrylamide to make final concentration of 65mg/l, at 50 DEG C, reacts 1h, stands, filters, after obtaining double purification treatment
Solution, survey solution in FeAlwaysMass concentration；
(3) the middle addition 18ml concentrated hydrochloric acids of solution (mass concentration is 135.52g/L) obtained to 100ml steps (2) make HCl
And FeAlwaysMass ratio be 0.55, add stabilizer the aqueous solution, (stabilizer is 2.14g silicic acid and 1.2g acetic acid) makes stabilizer
With FeAlwaysMol ratio=0.2, at 60 DEG C, under 100rpm stirrings, with flow as 0.1m3/ h is passed through air oxidation；
(4) molar content of solution ferrous ions is regularly determined in air event is passed through, when solution ferrous ions
When accounting for the 40% of the total molar content of iron, stopping is passed through air, adds 8.5g NaClO3Continue to aoxidize remaining ferrous ion, directly
To in solution without ferrous ion, the transparent poly-iron chloride liquid of 125ml yellowish-brown is obtained.Product can be with stable existence 10
Individual month.
Embodiment 3
A kind of method that poly-iron chloride is prepared by iron and steel pickling waste liquid, comprises the following steps：
(1) pretreatment of iron and steel pickling waste liquid：Iron and steel pickling waste liquid is taken, scrap iron skin reduction ferric iron is added, makes scrap iron skin
Mass content is 1%, is stirred, and places 2h；
(2) double purification treatment：Under agitation, the pH of pretreated iron and steel pickling waste liquid is adjusted with aqueous sodium carbonate
=4, add polyacrylamide to make final concentration of 45mg/l, at 40 DEG C, 3h is reacted, stand, filter, after obtaining double purification treatment
Solution, surveys Fe in solutionAlwaysMass concentration；
(3) the middle addition 14ml concentrated hydrochloric acids of solution (mass concentration is 161.84g/L) obtained to 100ml steps (2) make HCl
And FeAlwaysMass ratio be 0.45, add stabilizer the aqueous solution (stabilizer is 7.5g citric acids), make stabilizer and FeAlwaysRub
That ratio=0.30, at 15 DEG C, under 300rpm stirrings, with flow as 0.08m3/ h is passed through air oxidation；
Citric acid is substituted with phosphoric acid or disodium-hydrogen, other same the present embodiment prepare corresponding yellowish-brown transparent
Poly-iron chloride liquid.
(4) molar content of solution ferrous ions is regularly determined in air event is passed through, when solution ferrous ions
When accounting for the 30% of the total molar content of iron, stopping is passed through air, adds 14g H2O2Continue to aoxidize remaining ferrous ion, Zhi Daorong
Without untill ferrous ion in liquid, the transparent poly-iron chloride liquid of 132.5ml yellowish-brown is obtained.Product can be with stable existence 6
Month.
Embodiment 4
A kind of method that poly-iron chloride is prepared by iron and steel pickling waste liquid, comprises the following steps：
(1) pretreatment of iron and steel pickling waste liquid：Iron and steel pickling waste liquid is taken, iron reduction ferric iron is added, makes iron filings quality
Content is 0.6%, is stirred, and places 6h；
(2) double purification treatment：Under agitation, pretreated iron and steel pickling waste liquid is adjusted with sodium bicarbonate aqueous solution
PH=8, adds polyacrylamide to make final concentration of 70mg/l, at 80 DEG C, reacts 1h, stands, filters, after obtaining double purification treatment
Solution, survey solution in FeAlwaysMass concentration；
(3) the middle addition 18ml concentrated hydrochloric acids of solution (mass concentration is 161.84g/L) obtained to 100ml steps (2) make HCl
And FeAlwaysMass ratio be 0.52, add stabilizer the aqueous solution (stabilizer is 3.15g sodium dihydrogen phosphates and 2.2g acetic acid), make
Stabilizer and FeAlwaysMol ratio=0.15, at 60 DEG C, under 400rpm stirrings, with flow as 0.2m3/ h is passed through air oxidation；
(4) molar content of solution ferrous ions is regularly determined in air event is passed through, when solution ferrous ions
When accounting for the 25% of the total molar content of iron, stopping is passed through air, adds 12.5g H2O2Continue to aoxidize remaining ferrous ion, until
Without untill ferrous ion in solution, the transparent poly-iron chloride liquid of 135.85ml yellowish-brown is obtained.Product can be with stable existence 8
Individual month.
Claims (7)
1. it is a kind of that the method for poly-iron chloride is prepared by iron and steel pickling waste liquid, it is characterized in that comprising the following steps：
(1) pretreatment of iron and steel pickling waste liquid：Iron and steel pickling waste liquid is taken, reducing agent reduction ferric iron is added, makes reducing agent quality
Content is 0.2%~1%, is stirred, and places 2-10h；
(2) double purification treatment：Under agitation, pH=4~8 of pretreated iron and steel pickling waste liquid are adjusted with alkali, addition is helped
Agent polyacrylamide makes final concentration of 45~70mg/l, at 40~80 DEG C, reacts 0.5-3h, stands, filters, and obtains at double purification
Solution after reason, surveys Fe in solutionAlwaysMass concentration；
(3) HCl and Fe is made to addition hydrochloric acid in the solution of step (2) acquisitionAlwaysMass ratio be 0.45-0.55, add stabilizer
The aqueous solution, make stabilizer and FeAlwaysMol ratio=0.12-0.30, at 15-70 DEG C, under 100-400rpm stirrings, be with flow
0.05~0.2m3/ h is passed through air oxidation；
(4) molar content of solution ferrous ions is regularly determined in air event is passed through, when solution ferrous ions account for FeAlways
Molar content 5%-40% when, stopping is passed through air, adds oxidant to continue to aoxidize remaining ferrous ion, until in solution
Untill without ferrous ion, the transparent poly-iron chloride liquid of yellowish-brown is obtained.
2. method according to claim 1, it is characterized in that step (1) the reducing agent mass content is 0.5%~1%.
3. method according to claim 1 and 2, it is characterized in that the reducing agent is iron filings or scrap iron skin.
4. method according to claim 1, it is characterized in that step (2) double purification is processed as：Under agitation, adjusted with alkali
PH=5~7 of pretreated iron and steel pickling waste liquid, add auxiliary agent to make final concentration of 50~65mg/l, at 50~65 DEG C, stirring
0.5-3h, filtering obtains solution after after-treatment, surveys Fe in solutionAlwaysMass concentration.
5. the method according to claim 1 or 4, it is characterized in that the alkali is NaOH, ammoniacal liquor, sodium carbonate or bicarbonate
Sodium.
6. method according to claim 1, it is characterized in that the stabilizer is acetic acid, citric acid, phosphoric acid, the hydrogen of phosphoric acid one
One or two in salt, dihydric phosphate and silicic acid.
7. method according to claim 1, it is characterized in that the oxidant is H2O2Or NaClO3。
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| CN106379976A (en) * | 2016-08-30 | 2017-02-08 | 无锡市新都环保科技有限公司 | Equipment and method for preparing water treatment agent through using acidic iron-containing wastewater |
| CN109250762A (en) * | 2017-07-13 | 2019-01-22 | 鞍钢股份有限公司 | A method of poly-ferric chloride is prepared with steel hydrochloric acid pickling waste water |
| CN107555486B (en) * | 2017-09-18 | 2021-07-27 | 唐山市斯瑞尔化工有限公司 | Preparation method of polyferric chloride solid and polyferric chloride solid |
| CN108033490A (en) * | 2017-12-12 | 2018-05-15 | 青岛市昌斯达环保科技有限公司 | A kind of production method and technique of high-performance poly-ferric chloride |
| CN110316766A (en) * | 2019-07-17 | 2019-10-11 | 中信环境技术（广州）有限公司 | A kind of method of two-stage oxidizing waste hydrochloric acid containing iron preparation chlorination iron product |
| CN110615485B (en) * | 2019-09-05 | 2022-03-25 | 中信环境技术（广州）有限公司 | Continuous production method and application of polyferric chloride |
| CN111153477A (en) * | 2020-01-07 | 2020-05-15 | 斯瑞尔环境科技股份有限公司 | Preparation method of powdery polyferric chloride solid |
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| CN1266819A (en) * | 1999-03-11 | 2000-09-20 | 中国科学院生态环境研究中心 | Flocculant of polyiron chloride prepared from waste hydrochloric acid as pickling liquid of iron and steel and its preparing process |
| CN101353795A (en) * | 2008-08-26 | 2009-01-28 | 湖南万容科技有限公司 | Method for extracting copper from printed circuit board acidic spent etching solution and preparing poly ferric chloride |
| US10435316B2 (en) * | 2010-09-30 | 2019-10-08 | Orange County Sanitation District | Chemical optimization during wastewater treatment, odor control and uses thereof |
| CN102863031A (en) * | 2011-07-06 | 2013-01-09 | 福建方明环保科技有限公司 | Method for utilizing iron and steel acid washing liquid to produce catalyst and method for treating sewage |
| CN105271435B (en) * | 2015-10-06 | 2017-08-25 | 聊城大学 | Seamless steel pipe pickle liquor prepares the production technology of polyaluminium ferric flocculant |
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