CN105502512B - A kind of method that iron oxide yellow is prepared by iron and steel pickling waste liquid - Google Patents
A kind of method that iron oxide yellow is prepared by iron and steel pickling waste liquid Download PDFInfo
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- CN105502512B CN105502512B CN201610084122.2A CN201610084122A CN105502512B CN 105502512 B CN105502512 B CN 105502512B CN 201610084122 A CN201610084122 A CN 201610084122A CN 105502512 B CN105502512 B CN 105502512B
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention discloses a kind of method that iron oxide yellow is prepared by iron and steel pickling waste liquid, comprise the following steps：(1) iron and steel pickling waste liquid is taken, reducing agent is added；(2) under agitation, pH is adjusted, auxiliary agent is added, 0.5 3h is reacted, is stood, is filtered, obtain the solution after double purification treatment；(3) solution of small part step (2) acquisition is taken, dilute with water adjusts pH, under stirring, is passed through air, obtains the liquid containing iron oxide yellow crystal seed；(4) under agitation, the solution that remaining step (2) is obtained is added water, blowing air oxidation, dry iron oxide yellow.The method of the present invention is processed iron and steel pickling waste liquid, and with the acid solution after removal of impurities as raw material, versatile iron oxide yellow has been obtained, realize the recycling of steel acid pickle, turn waste into wealth, the method for the present invention is simple to operate, low cost, whole process environmental protection, is easy to implement industrialization.
Description
Technical field
The present invention relates to a kind of method that iron oxide yellow is prepared by iron and steel pickling waste liquid.
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, it will be our faces to find a kind of effective method and recycle pickling iron and steel acid pickle to be allowed to be converted into the material of high added value
The urgent task faced.
Iron oxide yellow is a kind of general iron oxide material that has many uses, because iron oxide yellow has high coloring power, very strong
Light resistance, temperature tolerance, can protect material sensitive to UV light, be incomparable conventional pigment.Iron oxide yellow these
Excellent performance, makes it be obtained in many fields such as superior automobile finish paint, woodwork coating, transparent plastic and widely should
With.Currently, the iron oxide pigment variety of China's production is single, lacks characteristic, and added value of product is low, it is difficult in fierce market
Taken the course of its own in competition, therefore explore new synthetic route, the quality and class for improving product will be that developing ability of ferrous oxide industry faces
A major challenge.
With in world wide to global ecological environment, the attention of sustainable development and the development of new and high technology to synthesis
The need for material, acquisition raw material prepares iron oxide yellow from secondary resource will also turn into a focus of future studies.If energy
The recycling of Industry Waste accessory substance is promoted in China, can not only solve the acid pickle that current steel industry faces difficult
Problem, turn waste into wealth, while also for the development of iron oxide yellow provides more wide prospect.
The content of the invention
The problem that a large amount of pickle liquors faced the invention aims to solve current steel industry cannot be processed, carries
For a kind of method that iron oxide yellow is prepared by iron and steel pickling waste liquid.
Technical scheme is summarized as follows：
A kind of method that iron oxide yellow 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, contains quality
It is 0.2%~1% to measure, and is stirred, and places 8-14h；
(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 solution2+Concentration, and be by volume 1-4：6-9 points is two parts；
(3) preparation of iron oxide yellow crystal seed：The solution of small part step (2) acquisition is taken, dilute with water makes Fe2+=0.2~
0.6mol/l, adjusts pH=5.5~8.5, is 0.05~0.2m with flow under 100-400rpm stirrings at 5~40 DEG C3/h
Air is passed through, pH=3~6 of solution are oxidizing to, the liquid containing iron oxide yellow crystal seed is obtained；
(4) preparation of iron oxide yellow：Under agitation, the solution that remaining most of step (2) obtains is added water makes Fe2+'s
Concentration obtains solution one for 0.1~0.8mol/l, solution one is added to solution two is obtained in the liquid containing iron oxide yellow crystal seed, makes
Fe in liquid containing iron oxide yellow crystal seed2+Molal quantity accounts for Fe in solution two2+The 10%~50% of molal quantity, adjusting temperature is
60~95 DEG C, be 0.01~0.2m with flow under the conditions of pH=2.0~4.03/ h blowing airs aoxidize 4~20h, dry oxygen
Change iron oxide yellow.
The reducing agent is iron powder or scrap iron skin.
Step (1) described mass content is 0.3%~0.5%.
Step (2) double purification is processed as：PH=5~7 of pretreated iron and steel pickling waste liquid are adjusted with alkali, addition is helped
Agent makes final concentration of 50~65mg/l, at 50~65 DEG C, reacts 0.5-3h, stands, filters, and obtains molten after double purification treatment
Liquid, surveys Fe in solution2+Concentration.
The alkali is NaOH, ammoniacal liquor, sodium carbonate or sodium acid carbonate.
The auxiliary agent is polyacrylamide or poly-iron chloride.
Step (3) iron oxide yellow crystal seed is prepared as：The solution of small part step (2) acquisition is taken, dilute with water makes Fe2+=
0.2~0.6mol/l, adjusts pH=6.0~8.0, at 10~30 DEG C, under 200-400rpm stirrings, with flow as 0.08~
0.15m3/ h is passed through air, is oxidizing to pH=4~6 of solution, obtains the liquid containing iron oxide yellow crystal seed.
Step (4) iron oxide yellow is prepared as：Under agitation, the solution that remaining most of step (2) obtains is added water makes Fe2+
Concentration obtain solution one for 0.2~0.8mol/l, solution one is added in the liquid containing iron oxide yellow crystal seed to obtain solution two,
Make Fe in the liquid containing iron oxide yellow crystal seed2+Molal quantity accounts for Fe in solution two2+The 25%~40% of molal quantity, adjusts temperature
It is 75~90 DEG C, is 0.08~0.15m with flow under the conditions of pH=2.0~4.03/ h blowing airs aoxidize 6~16h, dry
Iron oxide yellow.
Advantages of the present invention：The present invention is processed iron and steel pickling waste liquid using a kind of easy impurity removal process, is obtained
Clear impurity content low iron content acid solution, and with the acid solution after removal of impurities as raw material, versatile oxidation has been obtained
Iron oxide yellow, realizes the recycling of steel acid pickle, turns waste into wealth, while environmental protection is called in active response world wide
Economic benefit higher is obtained, a kind of solution party is provided by the intractable problem of pickle liquor that steel industry faces
Method.The method of the present invention is simple to operate, low cost, whole process environmental protection, is easy to implement industrialization.
Brief description of the drawings
Fig. 1 is the XRD of iron oxide yellow obtained in embodiment 2.
Fig. 2 is the TEM figures of iron oxide yellow obtained in embodiment 2.
Fig. 3 is the SEM figures of iron oxide yellow obtained in embodiment 2.
Fig. 4 is the XRD of iron oxide yellow obtained in embodiment 5.
Fig. 5 is the TEM figures of iron oxide yellow obtained in embodiment 5.
Fig. 6 is the SEM figures of iron oxide yellow obtained in embodiment 5.
Specific embodiment
With reference to specific example, the present invention is described further, and example below is the skill in order that this area
Art personnel can be better understood from the present invention, but the present invention not imposed any restrictions.
Embodiment 1
A kind of method that iron oxide yellow 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 is added, makes mass content be 0.3%,
Stir, place 14h；
(2) double purification treatment：Under agitation, the pH of pretreated iron and steel pickling waste liquid is adjusted with sodium hydroxide solution
=5, add polyacrylamide to make final concentration of 45mg/l, at 40 DEG C, 1h is reacted, cooling, standing, filtering are obtained at double purification
Solution after reason, with the Fe in potassium bichromate solution volumetric solution2+Concentration is n (Fe2+)=1.923mol/l；
Solution 345ml after double purification is processed is by volume 3：7 points is two parts；
(3) preparation of iron oxide yellow crystal seed：The solution of small part (3 parts) step (2) acquisition is taken, dilute with water makes Fe2+=
0.3mol/l, pH=6.0 is adjusted with ammoniacal liquor, at 30 DEG C, under 400rpm stirrings, with flow as 0.08m3/ h is passed through air, oxygen
Change to the pH=4 of solution, obtain the liquid containing iron oxide yellow crystal seed；
(4) preparation of iron oxide yellow：Under agitation, the solution that most of (7 parts) step (2) obtain is added water makes Fe2+Concentration
For 0.3mol/l obtains solution one, solution one is added to solution two is obtained in the liquid containing iron oxide yellow crystal seed, make to contain iron oxide yellow
Fe in the liquid of crystal seed2+Molal quantity accounts for Fe in solution two2+The 10% of molal quantity, is warming up to 95 DEG C, and solution is controlled with weak aqua ammonia
Under the conditions of pH=3.0, with flow as 0.08m3/ h blowing airs aoxidize 6h, dry iron oxide yellow 39.4g；
Embodiment 2
A kind of method that iron oxide yellow 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, reduced iron powder is added, makes mass content be 0.2%,
Stir, place 8h；
2) double purification treatment：Under agitation, the pH of pretreated iron and steel pickling waste liquid is adjusted with aqueous sodium carbonate
=7, add polyacrylamide to make final concentration of 50mg/l, at 50 DEG C, 0.5h is reacted, cooling, standing, filtering obtain double purification
Solution after treatment, with the Fe in potassium bichromate solution volumetric solution2+Concentration is n (Fe2+)=1.998mol/l；
Solution 180ml after double purification is processed is by volume 4：6 points is two parts
(3) preparation of iron oxide yellow crystal seed：The solution of small part (4 parts) step (2) acquisition is taken, dilute with water makes Fe2+=
0.2mol/l, pH=8.0 is adjusted with sodium hydroxide solution, at 10 DEG C, under 200rpm stirrings, with flow as 0.15m3/ h is passed through
Air, is oxidizing to the pH=4 of solution, obtains the liquid containing iron oxide yellow crystal seed；
(4) preparation of iron oxide yellow：Under agitation, the solution that remaining major part (6 parts) step (2) obtains is added water makes Fe2+
Concentration obtain solution one for 0.2mol/l, solution one is added in the liquid containing iron oxide yellow crystal seed to obtain solution two, make to contain
There is Fe in the liquid of oxidation iron oxide seed crystal2+Molal quantity accounts for Fe in solution two2+The 25% of molal quantity, is warming up to 75 DEG C, in pH=
Under the conditions of 2.5, with flow as 0.15m3/ h blowing airs oxidation 16h obtains iron oxide yellow 20.8g.
Embodiment 3
A kind of method that iron oxide yellow is prepared by iron and steel pickling waste liquid, comprises the following steps：
(1) pretreatment of iron and steel pickling waste liquid：Take iron and steel pickling waste liquid, add reducing agent iron powder, make the mass content be
1%, stir, place 12h；
(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 65mg/l, at 65 DEG C, reacts 3h, and cooling, standing, filtering obtain double purification
Solution after treatment, with the Fe in potassium bichromate solution volumetric solution2+Concentration is n (Fe2+)=2.058mol/l；
Solution 350ml after double purification is processed is by volume 4：6 points is two parts；
(3) preparation of iron oxide yellow crystal seed：The solution of small part (4 parts) step (2) acquisition is taken, dilute with water makes Fe2+=
0.6mol/l, pH=5.5 is adjusted with ammoniacal liquor, at 5 DEG C, under 300rpm stirrings, with flow as 0.2m3/ h is passed through air, oxidation
To the pH=6 of solution, the liquid containing iron oxide yellow crystal seed is obtained；
(4) preparation of iron oxide yellow：Under agitation, the solution that remaining major part (6 parts) step (2) obtains is added water makes
Fe2+Concentration obtain solution one for 0.8mol/l, solution one is added in the liquid containing iron oxide yellow crystal seed to obtain solution two, make
Fe in liquid containing iron oxide yellow crystal seed2+Molal quantity accounts for Fe in solution two2+The 40% of molal quantity, is warming up to 90 DEG C, in pH=
Under the conditions of 4, with flow as 0.01m3/ h blowing airs are oxidizing to 20h, dry iron oxide yellow 43.5g.
Embodiment 4
A kind of method that iron oxide yellow is prepared by iron and steel pickling waste liquid, comprises the following steps：
(1) pretreatment of iron and steel pickling waste liquid：Take iron and steel pickling waste liquid, add reducing agent scrap iron skin, make the mass content be
0.2%, stir, place 13h；
(2) double purification treatment：Under agitation, pretreated iron and steel pickling waste liquid is adjusted with sodium hydrate aqueous solution
PH=4, adds poly-iron chloride to make final concentration of 70mg/l, at 80 DEG C, reacts 2h, and cooling, standing, filtering are obtained at double purification
Solution after reason, with the Fe in potassium bichromate solution volumetric solution2+Concentration is n (Fe2+)=1.913mol/l；
Solution 262ml after double purification is processed is by volume 1：9 points is two parts
(3) preparation of iron oxide yellow crystal seed：The solution of small part (1 part) step (2) acquisition is taken, dilute with water makes Fe2+=
0.5mol/l, pH=8.5 is adjusted with ammoniacal liquor, at 40 DEG C, under 100rpm stirrings, with flow as 0.05m3/ h is passed through air, oxygen
Change to the pH=3 of solution, obtain the liquid containing iron oxide yellow crystal seed；
(4) preparation of iron oxide yellow：Under agitation, the solution that remaining major part (9 parts) step (2) obtains is added water makes
Fe2+Concentration obtain solution one for 0.1mol/l, solution one is added in the liquid containing iron oxide yellow crystal seed to obtain solution two, make
Fe in liquid containing iron oxide yellow crystal seed2+Molal quantity accounts for Fe in solution two2+The 50% of molal quantity, is warming up to 60 DEG C, in pH=
Under the conditions of 2, with flow as 0.2m3/ h blowing airs aoxidize 4h, dry iron oxide yellow 35.6g；
Embodiment 5
A kind of method that iron oxide yellow is prepared by iron and steel pickling waste liquid, comprises the following steps：
(1) pretreatment of iron and steel pickling waste liquid：Take iron and steel pickling waste liquid, add reduced iron powder, make the mass content be
0.5%, stir, place 11h；
(2) removal of impurities：Under agitation, the pH=5.5 of pretreated iron and steel pickling waste liquid is adjusted with weak aqua ammonia, poly- third is added
Acrylamide makes final concentration of 65mg/l, at 60 DEG C, reacts 2.5h, and cooling, standing, filtering obtain the solution after double purification treatment,
With the Fe in potassium bichromate solution volumetric solution2+Concentration is n (Fe2+)=2.043mol/l；
Solution 399ml after double purification is processed is by volume 2：8 points is two parts
(3) preparation of iron oxide yellow crystal seed：The solution of small part (2 parts) step (2) acquisition is taken, dilute with water makes Fe2+=
0.5mol/l, pH=7.5 is adjusted with ammoniacal liquor, at 30 DEG C, under 300rpm stirrings, with flow as 0.14m3/ h is passed through air, oxygen
Change to the pH=6 of solution, obtain the liquid containing iron oxide yellow crystal seed；
(4) preparation of iron oxide yellow：Under agitation, the solution that remaining major part (8 parts) step (2) obtains is added water makes
Fe2+Concentration obtain solution one for 0.4mol/l, solution one is added in the liquid containing iron oxide yellow crystal seed to obtain solution two, make
Fe in liquid containing iron oxide yellow crystal seed2+Molal quantity accounts for Fe in solution two2+The 28% of molal quantity, is warming up to 90 DEG C, in pH=
Under the conditions of 6.5, with flow as 0.15m3/ h blowing airs are oxidizing to 7h and obtain iron oxide yellow 52.5g.
Claims (6)
1. it is a kind of that the method for iron oxide yellow 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 is added, makes mass content be 0.2%~1%,
Stir, place 8-14h；
(2) double purification treatment：Under agitation, pH=5~7 of pretreated iron and steel pickling waste liquid are adjusted with alkali, addition is helped
Agent makes final concentration of 50~65mg/l, at 50~65 DEG C, reacts 0.5-3h, stands, filters, and obtains molten after double purification treatment
Liquid, surveys Fe in solution2+Concentration, and be by volume 1-4：6-9 points is two parts；
(3) preparation of iron oxide yellow crystal seed：The solution of small part step (2) acquisition is taken, dilute with water makes Fe2+=0.2~
0.6mol/l, adjusts pH=5.5~8.5, is 0.05~0.2m with flow under 100-400rpm stirrings at 5~40 DEG C3/h
Air is passed through, pH=3~6 of solution are oxidizing to, the liquid containing iron oxide yellow crystal seed is obtained；
(4) preparation of iron oxide yellow：Under agitation, the solution that remaining most of step (2) obtains is added water makes Fe2+Concentration
For 0.1~0.8mol/l obtains solution one, solution one is added in the liquid containing iron oxide yellow crystal seed to obtain solution two, make containing
Fe in the liquid of iron oxide yellow crystal seed2+Molal quantity accounts for Fe in solution two2+The 10%~50% of molal quantity, regulation temperature be 60~
95 DEG C, be 0.01~0.2m with flow under the conditions of pH=2.0~4.03/ h blowing airs aoxidize 4~20h, dry iron oxide
It is yellow.
2. method according to claim 1, it is characterized in that the reducing agent is iron powder or scrap iron skin.
3. method according to claim 1 and 2, it is characterized in that step (1) described mass content is 0.3%~0.5%.
4. method according to claim 1, it is characterized in that the alkali is NaOH, ammoniacal liquor, sodium carbonate or sodium acid carbonate.
5. method according to claim 1, it is characterized in that the auxiliary agent is polyacrylamide or poly-iron chloride.
6. method according to claim 1, it is characterized in that step (3) iron oxide yellow crystal seed is prepared as：Take small part step
Suddenly the solution that (2) obtain, dilute with water makes Fe2+=0.2~0.6mol/l, adjusts pH=6.0~8.0, at 10~30 DEG C,
It is 0.08~0.15m with flow under 200-400rpm stirrings3/ h is passed through air, is oxidizing to pH=4~6 of solution, obtains containing aerobic
Change the liquid of iron oxide seed crystal.
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| CN107585791A (en) * | 2017-09-28 | 2018-01-16 | 福州琪宁精细化工有限公司 | A kind of preparation method of iron oxide |
| CN108455681B (en) * | 2018-02-05 | 2020-07-14 | 吉林建筑大学 | Method for preparing iron oxide yellow pigment by using iron and aluminum-containing industrial wastewater |
| CN108640159A (en) * | 2018-02-27 | 2018-10-12 | 天津丹兴科技有限责任公司 | A kind of pickling sludge and pickle liquor harmless resource utilization integrated conduct method |
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| DE19812260A1 (en) * | 1998-03-20 | 1999-09-23 | Bayer Ag | Production of iron oxide pigments from dilute acid formed in manufacture of titanium dioxide |
| CN101649130B (en) * | 2009-09-03 | 2012-05-30 | 浙江大学 | Method for preparing ferric oxide yellow pigment by waste iron hydrochloric acid lotion |
| CN103145194B (en) * | 2011-12-06 | 2016-03-30 | 北京三聚环保新材料股份有限公司 | A kind of method utilizing by-product of white titanium pigment to prepare iron oxide yellow |
| CN103145193B (en) * | 2011-12-06 | 2015-08-26 | 北京三聚环保新材料股份有限公司 | A kind of by-product of white titanium pigment prepares the method for iron oxide yellow |
| CN102616862A (en) * | 2012-02-21 | 2012-08-01 | 升华集团德清华源颜料有限公司 | Method for preparing nano-sized transparent yellow iron oxide pigments |
| CN104512933A (en) * | 2013-09-28 | 2015-04-15 | 天津市大港华明化工厂 | Method for producing iron oxide yellow and iron oxide red by using waste hydrochloric acid solution |
| CN104478001A (en) * | 2014-11-20 | 2015-04-01 | 周淑华 | Method for producing iron oxide yellow from acidic waste water in titanium dioxide industry |
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